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CN110057936A - A kind of content assaying method of vitamin E - Google Patents

A kind of content assaying method of vitamin E Download PDF

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Publication number
CN110057936A
CN110057936A CN201910373613.2A CN201910373613A CN110057936A CN 110057936 A CN110057936 A CN 110057936A CN 201910373613 A CN201910373613 A CN 201910373613A CN 110057936 A CN110057936 A CN 110057936A
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solution
vitamin
standard
concentration
scale
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Inventor
吴以岭
吴相君
吴瑞
贾振华
郑晓杰
闫琳
王光路
李晓燕
孙亚琴
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Shijiazhuang Yiling Pharmaceutical Co Ltd
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Shijiazhuang Yiling Pharmaceutical Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Cosmetics (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention provides a kind of methods of content of vitamin E in measurement Vitamin E preparation, and this method processing sample is simple, and required time saves 6-8 times than national standard, and in the detection process, without using any solvent for having pollution, and accuracy is high.

Description

A kind of content assaying method of vitamin E
Technical field
The invention belongs to analysis of pharmaceutical dosage forms fields, are specifically related to a kind of Vitamin E preparation content assaying method.
Background technique
Vitamin E is a kind of liposoluble vitamin, also known as tocopherol, is one of most important antioxidant.Vitamin E exists Effect is the most extensive in human body, all bigger than any nutrient, therefore has the title of " escorting ambassador ".Have in body good Inoxidizability, i.e. reduction cell senescence.The effect of integrality of holding red blood cell, promotes cell to synthesize, antipollution, antisterility.
Be deficient in vitamin E, will lead to atherosclerosis, blood concentration anaemia, cancer, other old leg rows such as cataract Lesion disease；Form scar；Tooth can be made to turn to be yellow；Cause myopia；Cause disability, retarded child；Cause male sexual dysfunction； Hypertrophy of the prostate etc..Vitamin E can treat or prevent following illness:
1, atherosclerosis is treated
Daily intake 100 milligrams of vitamin or more, can slow down it is light, in or severe coronary atherosclerosis progress.According to another Report takes 00 milligram of vitamin E2 and 90,000 unit of vitamin A to arteriosclerosis patient, headache after 6 to 10 weeks, insomnia, dizzy The symptoms such as dizzy, tinnitus can mitigate, blood pressure decline, lipid cholesterol decline.
2, congestive cardiac insufficiency and angina pectoris are treated, gives daily vitamin E2 00 milligram to 400 to this kind of patient Milligram, can be such that exercise load increases, and angina pectoris disappears, and has diuresis.
3, vitamin E, which has control growth of tumour cell, to be shown to the preventive and therapeutic effect inside and outside experiment of tumour, reduces or prolongs The effect that slow in-vivo tumour occurs.Epidemic disease data is also shown, body vitamin E intake and tumour negative correlation.
4, vitamin E and gynecological disease take vitamin E soft capsules can cure some women place intrauterine device after occur go out Blood or menorrhalgia.Method is: oral vitamin E100 milligrams every other day, 7 days are 1 course for the treatment of, 1 to 3 courses for the treatment of of general treatment. Separately it has been reported that vitamin E can treat immune infertility, anovulatory infertility and habitual abortion.
Structure is complicated for vitamin E, and isomers type is more, and analysis measurement is difficult, and existing measuring method includes: spectrophotometric A variety of detection methods such as method, fluorescence method, high performance liquid chromatography, gas chromatography, double wave voltage method, oscillographic method, various detections It is had a certain difference between method, needs to find a kind of standard determination method quickly, accurate, easy.
The detection method that national standard (5009. 82-2016 of GB) uses at present is sample through saponification, extraction, washing, dense It after contracting, is detected using high-efficient liquid phase technique, that there is sample processing times is long for this method, expends that reagent is more, accuracy is opposite The problems such as lower.
Summary of the invention
The present invention provides a kind of method of content of vitamin E in measurement Vitamin E preparation, this method handles sample letter Single, required time saves 6-8 times than national standard, and in the detection process, without using any solvent for having pollution, and accuracy is high.
The present invention provides a kind of content assaying method of Vitamin E preparation, method includes the following steps:
A, the preparation of standard solution: configuring the vitamin E titer of various concentration, and vitamin E standard system is made in prepared before use Column working solution；
B, the preparation of test solution: taking vitamin E after saponification, neutralization, extraction, and filtering takes subsequent filtrate for high-efficient liquid phase color Spectrum measurement；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, draws mark Directrix curve calculates linear regression equation；
D, chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.5-1.2mL/min；Column temperature: 10-35 DEG C；Detection Wavelength: 292-298 nm；Sampling volume: 5-20 μ L, by the test solution of step B through high performance liquid chromatograph analyze to get.
The content assaying method preferably includes following steps:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing Vitamin E preparation content, and warm water is added and mixes, adds ascorbic acid and 2, 6- di-tert-butyl p-cresol mixes, and sequentially adds dehydrated alcohol, potassium hydroxide solution, and edged shaking in side mixes after saponification；It will Saponification liquor adds hydrochloric acid solution to neutralize, and mixes, and adds methanol dilution to scale, shakes up, filter, subsequent filtrate is taken to survey for high performance liquid chromatography It is fixed；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures peak Area draws standard curve by abscissa of standard test liquid concentration, calculates linear regression equation using peak area as ordinate；
D, chromatographic condition: chromatographic column is C18 column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area by 10 μ L, uses External standard method calculates its concentration by above-mentioned standard curve to obtain the final product.
The content assaying method preferably includes following steps:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing 1.0-2.0g sample, and 20-30 mL warm water is added, and mixes, adds 1.0-1.5g Ascorbic acid and 0.1-0.2g 2,6-di-tert-butyl p-cresol mix, and 30-40 mL dehydrated alcohol is added, and 10-15 mL is added Potassium hydroxide solution, the shaking of side edged, 80-85 DEG C of constant temperature is saponified 30min after mixing, is cooled to room with cold water immediately after saponification Saponification liquor is transferred in 100 mL brown volumetric flasks by temperature, and washs conical flask with 30-40mL moisture time, and washing lotion is also transferred to In measuring bottle, water is added to be settled to scale, shaken up, precision measures above-mentioned saponification liquor 1-3mL into 100 mL brown measuring bottles, adds hydrochloric acid molten Liquid 1-3 mL is mixed, and is added methanol dilution to scale, is shaken up, take this solution filter membrane, subsequent filtrate is taken to survey for high performance liquid chromatography It is fixed；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures phase The peak area answered draws standard curve by abscissa of standard test liquid concentration, calculates linear regression using peak area as ordinate Equation；
D, chromatographic condition: chromatographic column is C18 column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area by 10 μ L, uses External standard method calculates its concentration by above-mentioned standard curve.
The content assaying method can also preferably comprise following steps:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing 1.0g sample, and 20 mL warm water are added, and mixes, add 1.0g ascorbic acid and 0.1g 2,6-di-tert-butyl p-cresol mixes, and 30 mL dehydrated alcohols are added, and 10 mL potassium hydroxide solutions, the vibration of side edged is added It shakes, in 80 DEG C of water bath with thermostatic control concussion saponification 30min after mixing, is cooled to room temperature immediately with cold water after saponification, saponification liquor is transferred to In 100 mL brown volumetric flasks, and conical flasks are washed with 30 mL moisture time, washing lotion is also transferred in measuring bottle, and water is added to be settled to quarter Degree, shakes up, and precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds 1.9 mL of hydrochloric acid solution, mixes, adds methanol It is diluted to scale, is shaken up, this solution is taken to cross 0.22 μm of organic system filter membrane, subsequent filtrate is taken to measure for high performance liquid chromatography；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures phase The peak area answered draws standard curve by abscissa of standard test liquid concentration, calculates linear regression using peak area as ordinate Equation；
D, chromatographic condition: chromatographic column is C18 column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area by 10 μ L, uses External standard method calculates its concentration by above-mentioned standard curve.
The content assaying method can also preferably comprise following steps:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing 1.5g sample, and 30mL warm water is added, and mixes, add 1.5g ascorbic acid and 0.2g 2,6-di-tert-butyl p-cresol mixes, and 40 mL dehydrated alcohols are added, and 15 mL potassium hydroxide solutions, the vibration of side edged is added It shakes, in 85 DEG C of water bath with thermostatic control concussion saponification 30min after mixing, is cooled to room temperature immediately with cold water after saponification, saponification liquor is transferred to In 100 mL brown volumetric flasks, and conical flasks are washed with 40 mL moisture time, washing lotion is also transferred in measuring bottle, and water is added to be settled to quarter Degree, shakes up, and precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds 1.5 mL of hydrochloric acid solution, mixes, adds methanol It is diluted to scale, is shaken up, this solution is taken to cross 0.22 μm of organic system filter membrane, subsequent filtrate is taken to measure for high performance liquid chromatography；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures phase The peak area answered draws standard curve by abscissa of standard test liquid concentration, calculates linear regression using peak area as ordinate Equation；
D, chromatographic condition: chromatographic column is C18 column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area by 10 μ L, uses External standard method calculates its concentration by above-mentioned standard curve.
The preparation of step B test solution described in preferred the method for the present invention operates under light protected environment, the vessel used Oxidizing substance must not be contained.
Application of the content assaying method of the present invention in health care product of the measurement containing vitamin E, drug or food, the guarantor Strong product are made of D- α-D-α-tocopherol acetate, gelatin, purified water, corn oil, glycerol.
In order to confirm that the stability, accuracy, feasibility of the method for the present invention have carried out following experimental study:
1 principle: the vitamin E in sample is after saponification, neutralization, extraction, the separation of C18 Reversed Phase High Performance, ultraviolet inspection Survey device detection, quantified by external standard method.
2 reagents and material: unless otherwise indicated, this method agents useful for same is that analysis is pure, and water is ultrapure water.
3 preparation of reagents
3.1 potassium hydroxide solutions (50g/100g): weighing 50g potassium hydroxide, and the dissolution of 50mL water is added and is stored in poly- after cooling In ethylene bottle.
3.2 hydrochloric acid solutions: taking hydrochloric acid 10mL, and water is added to make to be diluted to 100mL, shake up to get.
4 vitamin E standard items: alpha-tocopherol (C29H50O2, No. CAS: 10191-41-0): purity >=95%, or through state Family authenticates and authorizes the standard substance of standard substance certificate.
5 standard solution are prepared
5.1 vitamin E Standard Stock solutions (1.00mg/mL): alpha-tocopherol 50.0mg is accurately weighed, is dissolved with dehydrated alcohol Afterwards, it is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is about 1.00mg/mL.After solution is sealed ,- It is kept in dark place at 20 DEG C, validity period 6 months.Solution is risen again to 20 DEG C before use, and carries out concentration correction.
5.2 vitamin E standard solution intermediate fluids: the accurate vitamin E Standard Stock solutions 10.00mL that draws is in 50 milliliters In brown volumetric flask, with methanol constant volume to scale, the concentration of alpha-tocopherol is 200 μ g/mL in this solution.It is protected from light at -20 DEG C It saves, two weeks validity period.
5.3 vitamin E standard series working solutions: accurate absorption 0.50 mL of vitamin E standard solution intermediate fluid, 1.00 ML, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are in 10mL brown volumetric flask, with methanol constant volume to scale, the standard Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in series, 100.0 μ g/mL, prepared before use.
6 instrument and equipments
6.1 assay balances: sensibility reciprocal 0.01mg.
6.2 thermostatic control oscillator vibration.
6.3 ultraviolet specrophotometer.
6.4 high performance liquid chromatographs: band UV detector.
7 analytical procedures
The preparation of 7.1 samples
20 vitamin E capsules are taken, content is poured out, is uniformly mixed, is stored in sample bottle, is protected from light refrigeration, measures as early as possible.
7.2 sample pretreating
Warning: all vessel used must not contain oxidizing substance；Ultraviolet lighting should be avoided in treatment process, is protected from light behaviour as far as possible Make；Extraction process should operate in vent cabinet.
Accurately weighed each 1.0g sample of three batches of samples is respectively placed in 150 mL stuffed conical flasks, and 20 mL warm water are added, and is mixed It is even, 1.0g ascorbic acid and 0.1g 2,6-di-tert-butyl p-cresol are added, is mixed, 30 mL dehydrated alcohols are added, is added 10 ML potassium hydroxide solution, the shaking of side edged use cold water in 80 DEG C of water bath with thermostatic control concussion saponification 30min after mixing immediately after saponification It is cooled to room temperature.Saponification liquor is transferred in 100 mL brown volumetric flasks, and washs conical flasks with 30 mL moisture time, washing lotion is also It is transferred in measuring bottle, water is added to be settled to scale, shake up.Precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds salt 1.9 mL of acid solution is mixed, is added methanol dilution to scale, shake up, take this solution to cross 0.22 μm of organic system filter membrane, subsequent filtrate is taken to supply High performance liquid chromatography measurement.
8 chromatography reference conditions
Chromatography reference conditions are listed below:
8.1 chromatographic columns: C18 column (column length 250mm, internal diameter 4.6mm, 5 μm of partial size)
8.2 column temperatures: 20 DEG C
8.3 mobile phases: methanol
8.4 flow velocitys: 0.8 mL/min
8.5 ultraviolet detection wavelength: 294nm
8.6 sample volumes: 10 μ L
The production of 9 standard curves
This law uses quantified by external standard method.Vitamin E standard series working solution is injected separately into high performance liquid chromatograph, is measured Corresponding peak area draws standard curve by abscissa of standard test liquid concentration using peak area as ordinate, calculates straight line and returns Return equation.
The measurement of 10 samples
Sample is analyzed through high performance liquid chromatograph, measures peak area, calculates its concentration by above-mentioned standard curve using external standard method. In continuous mode, it is proposed that stability of every 10 samples of measurement with a standard solution or standard substance inspection apparatus.
The statement of 11 analysis results
The content of vitamin E is calculated as follows in sample:
In formula:
The content of vitamin E in X-sample, mg/；
C-calculates to obtain the concentration of vitamin E, μ g/mL in test solution by standard curve；
V1-sample constant volume, mL；
V2-measurement solution constant volume, mL；
V3-measurement solution dilutes sample volume, mL；
M-is averaged loading amount, and g/；
W-sample sample weighting amount, g；
Calculated result retains three effective digitals.
Compared with the content of 82-2016 method of GB5009. measurement vitamin E, there are following advantages by the present invention:
1, the sample treatment used in the present invention eliminates the operating process such as extraction, washing, concentration compared with national standard method, Method is simple, easy to operate, reproducible, eliminates the difference between operator；
2, the method applied in the present invention is time saving, laborsaving, reduces chemical levels, reduces environmental pollution；
3, through to same batch of sample detection, this method measurement result is the 101% of additive amount, national standard method is additive amount 96.0%, illustrate that accuracy of measurement of this method for vitamin E in sample improves.
The preparation of vitamin E soft capsule: [raw material] D- α-D-α-tocopherol acetate；It is [auxiliary material] gelatin, purified water, corn oil, sweet Oil；[production technology] this product is processed into through main techniques such as mixing, pelleting, packagings.
Embodiment 1:
Vitamin E soft capsule assay
The preparation of test solution: weighing 1.005g vitamin E soft capsule content, and 15 mL warm water are added, and mixes, adds 1.5g ascorbic acid and 0.1g 2,6-di-tert-butyl p-cresol mix, and 30 mL dehydrated alcohols are added, and 10 mL hydroxides are added Potassium solution, the shaking of side edged, 80 DEG C of constant temperature are saponified 30min after mixing, are cooled to room temperature immediately with cold water after saponification, by saponification liquor It is transferred in 100mL brown volumetric flask, and washs conical flask with 30 moisture time, washing lotion is also transferred in measuring bottle, and water is added to be settled to Scale shakes up, and precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds hydrochloric acid solution 1.5mL, mixes, adds methanol It is diluted to scale, is shaken up, this solution filter membrane is taken, subsequent filtrate is taken to measure for high performance liquid chromatography.
The production of standard curve: standard solution is prepared, and vitamin E Standard Stock solutions (1.00mg/mL): is accurately weighed Alpha-tocopherol 50.0mg after being dissolved with dehydrated alcohol, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration About 1.00mg/mL.It after solution is sealed, is kept in dark place at -20 DEG C, validity period 6 months, solution is risen again to 20 before use DEG C, and carry out concentration correction；Vitamin E standard solution intermediate fluid: it is accurate draw vitamin E Standard Stock solutions 10.00mL in In 50 milliliters of brown volumetric flasks, with methanol constant volume to scale, the concentration of alpha-tocopherol is 200 μ g/mL in this solution.At -20 DEG C Under be kept in dark place, two weeks validity period；Vitamin E standard series working solution: accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL use methanol constant volume in 10mL brown volumetric flask To scale, Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL in the standard series, 80.0 μ g/mL, 100.0 μ g/mL, prepared before use.Vitamin E standard series working solution is injected separately into high-efficient liquid phase color In spectrometer, corresponding peak area is measured, using peak area as ordinate, it is bent to draw standard using standard test liquid concentration as abscissa Line calculates linear regression equation.
Chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area by 10 μ L, uses It is 103.0mg/ that external standard method, which calculates its content by above-mentioned standard curve,.
Embodiment 2:
Vitamin E soft capsule assay
The preparation of test solution: weighing 1.015g vitamin E soft capsule content, and 20 mL warm water are added, and mixes, adds 1.0g ascorbic acid and 0.1g 2,6-di-tert-butyl p-cresol mix, and 30 mL dehydrated alcohols are added, and 10 mL hydroxides are added Potassium solution, the shaking of side edged are cooled to room with cold water immediately after saponification in 80 DEG C of water bath with thermostatic control concussion saponification 30min after mixing Temperature, saponification liquor are transferred in 100 mL brown volumetric flasks, and wash conical flasks with 30 mL moisture time, and washing lotion is also transferred to measuring bottle In, add water to be settled to scale, shake up, precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds hydrochloric acid solution 1.9 ML is mixed, is added methanol dilution to scale, shake up, take this solution to cross 0.22 μm of organic system filter membrane, take subsequent filtrate for high-efficient liquid phase color Spectrum measurement；
The production of standard curve: standard solution is prepared, and vitamin E Standard Stock solutions (1.00mg/mL): accurately weighs α-life Phenol 50.0mg is educated, after being dissolved with dehydrated alcohol, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is about 1.00mg/mL.It after solution is sealed, is kept in dark place at -20 DEG C, validity period 6 months, solution is risen again to 20 DEG C before use, And carry out concentration correction；Vitamin E standard solution intermediate fluid: the accurate vitamin E Standard Stock solutions 10.00mL that draws is in 50 In milliliter brown volumetric flask, with methanol constant volume to scale, the concentration of alpha-tocopherol is 200 μ g/mL in this solution.At -20 DEG C It is kept in dark place, two weeks validity period；Vitamin E standard series working solution: accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL use methanol constant volume in 10mL brown volumetric flask To scale, Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL in the standard series, 80.0 μ g/mL, 100.0 μ g/mL, prepared before use.Vitamin E standard series working solution is injected separately into high-efficient liquid phase color In spectrometer, corresponding peak area is measured, using peak area as ordinate, it is bent to draw standard using standard test liquid concentration as abscissa Line calculates linear regression equation；
Chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.6mL/min；Column temperature: 30 DEG C；Detection wavelength: 292 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area, using external standard by 10 μ L It is 102.4mg/ that method, which calculates its content by above-mentioned standard curve,.
Embodiment 3:
Vitamin E soft capsule assay
The preparation of test solution: weighing 1.505g vitamin E soft capsule content, and 30mL warm water is added, and mixes, adds 1.5g ascorbic acid and 0.2g 2,6-di-tert-butyl p-cresol mix, and 40 mL dehydrated alcohols are added, and 15 mL hydroxides are added Potassium solution, the shaking of side edged are cooled to room with cold water immediately after saponification in 85 DEG C of water bath with thermostatic control concussion saponification 30min after mixing Temperature, saponification liquor are transferred in 100 mL brown volumetric flasks, and wash conical flasks with 40 mL moisture time, and washing lotion is also transferred to measuring bottle In, add water to be settled to scale, shake up, precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds hydrochloric acid solution 1.5 ML is mixed, is added methanol dilution to scale, shake up, take this solution to cross 0.22 μm of organic system filter membrane, take subsequent filtrate for high-efficient liquid phase color Spectrum measurement；
The production of standard curve: standard solution is prepared, and vitamin E Standard Stock solutions (1.00mg/mL): accurately weighs α-life Phenol 50.0mg is educated, after being dissolved with dehydrated alcohol, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is about 1.00mg/mL.It after solution is sealed, is kept in dark place at -20 DEG C, validity period 6 months, solution is risen again to 20 DEG C before use, And carry out concentration correction；Vitamin E standard solution intermediate fluid: the accurate vitamin E Standard Stock solutions 10.00mL that draws is in 50 In milliliter brown volumetric flask, with methanol constant volume to scale, the concentration of alpha-tocopherol is 200 μ g/mL in this solution.At -20 DEG C It is kept in dark place, two weeks validity period；Vitamin E standard series working solution: accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL use methanol constant volume in 10mL brown volumetric flask To scale, Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL in the standard series, 80.0 μ g/mL, 100.0 μ g/mL, prepared before use.Vitamin E standard series working solution is injected separately into high-efficient liquid phase color In spectrometer, corresponding peak area is measured, using peak area as ordinate, it is bent to draw standard using standard test liquid concentration as abscissa Line calculates linear regression equation；
Chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 1.0mL/min；Column temperature: 15 DEG C；Detection wavelength: 298 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area, using external standard by 10 μ L It is 101.2mg/ that method, which calculates its content by above-mentioned standard curve,.
Comparative example 1: it takes with a collection of vitamin E soft capsule (364 mg/g of vitamin E theoretical content amount), respectively with national standard side Method and the method for the present invention carry out the assay of vitamin E, compare the reapective features of two methods, specific as follows:
By the above test result it is found that the method for the present invention used time is short, it is thus only necessary to which 1 hour, national standard method needed 8 hours；This hair Bright method organic solvent uses opposite national standard method less, effectively reduces environmental pollution, and reduces testing cost；And the present invention Method measured value is more accurate, has reached 103%, and national standard method is only 96%, in conclusion the present invention measures vitamin E Method and existing national standard method have measurement result is more acurrate, the used time is shorter, it is more friendly to environment, can greatly reduce Testing cost produces significant technical effect.

Claims (9)

1. a kind of content assaying method of Vitamin E preparation, which is characterized in that method includes the following steps:
A, the preparation of standard solution: configuring the vitamin E titer of various concentration, and vitamin E standard system is made in prepared before use Column working solution；
B, the preparation of test solution: taking Vitamin E preparation appropriate, and after saponification, neutralization, extraction, filtering takes subsequent filtrate i.e. ?；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, draws mark Directrix curve calculates linear regression equation；
D, chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.5-1.2mL/min；Column temperature: 10-35 DEG C；Detection Wavelength: 292-298 nm；Sampling volume: 5-20 μ L, by the test solution of step B through high performance liquid chromatograph analyze to get.
2. the content assaying method of Vitamin E preparation according to claim 1, it is characterised in that this method includes following step It is rapid:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing Vitamin E preparation content, and warm water is added and mixes, adds ascorbic acid and 2, 6- di-tert-butyl p-cresol mixes, and sequentially adds dehydrated alcohol, potassium hydroxide solution, and edged shaking in side mixes after saponification, soap It is cooled to room temperature immediately with cold water after change；Saponification liquor plus hydrochloric acid solution are neutralized, is mixed, is added methanol dilution to scale, shake up, mistake Filter takes subsequent filtrate to measure for high performance liquid chromatography；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures peak Area draws standard curve by abscissa of standard test liquid concentration, calculates linear regression equation using peak area as ordinate；
D, chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area, using external standard by 10 μ L Method calculates its concentration by above-mentioned standard curve to obtain the final product.
3. content assaying method according to claim 1, which is characterized in that method includes the following steps:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing 1.0-2.0g sample, and 20-30 mL warm water is added, and mixes, adds 1.0-1.5g Ascorbic acid and 0.1-0.2g 2,6-di-tert-butyl p-cresol mix, and 30-40 mL dehydrated alcohol is added, and 10-15 mL is added Potassium hydroxide solution, the shaking of side edged, 80-85 DEG C of constant temperature is saponified 30min after mixing, is cooled to room with cold water immediately after saponification Saponification liquor is transferred in 100 mL brown volumetric flasks by temperature, and washs conical flasks with 30-40mL moisture time, and washing lotion is also transferred to In measuring bottle, water is added to be settled to scale, shaken up, precision measures above-mentioned saponification liquor 1-3mL into 100 mL brown measuring bottles, adds hydrochloric acid molten Liquid 1-3 mL is mixed, and is added methanol dilution to scale, is shaken up, take this solution filter membrane, subsequent filtrate is taken to survey for high performance liquid chromatography It is fixed；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures phase The peak area answered draws standard curve by abscissa of standard test liquid concentration, calculates linear regression using peak area as ordinate Equation；
D, chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area, using external standard by 10 μ L Method calculates its concentration by above-mentioned standard curve.
4. content assaying method according to claim 1, which is characterized in that content assaying method described in this method include with Lower step:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing 1.0g sample, and 20 mL warm water are added, and mixes, add 1.0g ascorbic acid and 0.1g 2,6-di-tert-butyl p-cresol mixes, and 30 mL dehydrated alcohols are added, and 10 mL potassium hydroxide solutions, the vibration of side edged is added It shakes, in 80 DEG C of water bath with thermostatic control concussion saponification 30min after mixing, is cooled to room temperature immediately with cold water after saponification, saponification liquor is transferred to In 100 mL brown volumetric flasks, and conical flasks are washed with 30 mL moisture time, washing lotion is also transferred in measuring bottle, and water is added to be settled to quarter Degree, shakes up, and precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds 1.9 mL of hydrochloric acid solution, mixes, adds methanol It is diluted to scale, is shaken up, this solution is taken to cross 0.22 μm of organic system filter membrane, subsequent filtrate is taken to measure for high performance liquid chromatography；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures phase The peak area answered draws standard curve by abscissa of standard test liquid concentration, calculates linear regression using peak area as ordinate Equation；
D, chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area, using external standard by 10 μ L Method calculates its concentration by above-mentioned standard curve.
5. content assaying method according to claim 1, which is characterized in that content assaying method described in this method include with Lower step:
A, the preparation of standard solution: a, vitamin E Standard Stock solutions: precision weighs alpha-tocopherol 50.0mg, uses dehydrated alcohol It after dissolution, is transferred in 50mL brown volumetric flask, is settled to scale, this solution concentration is 1.00mg/mL；After solution is sealed, It is kept in dark place at -20 DEG C, validity period 6 months；Solution is risen again to 20 DEG C before use, and carries out concentration correction；B, vitamin E standard solution intermediate fluid is prepared: the accurate vitamin E Standard Stock solutions 10.00mL that draws is used in 50 milliliters of brown volumetric flasks Methanol constant volume is to scale, and the concentration of alpha-tocopherol is 200 μ g/mL in this solution；It is kept in dark place at -20 DEG C, half of validity period Month；D, vitamin E standard series working solution: it is accurate to draw vitamin E standard solution intermediate fluid 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL are respectively placed in 10mL brown volumetric flask, with methanol constant volume to scale, the mark Vitamin E levels are 10.0 μ g/mL, 20.0 μ g/mL, 40.0 μ g/mL, 60.0 μ g/mL, 80.0 μ g/mL in quasi- series, 100.0 μ g/mL, prepared before use；
B, the preparation of test solution: weighing 1.5g sample, and 30mL warm water is added, and mixes, add 1.5g ascorbic acid and 0.2g 2,6-di-tert-butyl p-cresol mixes, and 40 mL dehydrated alcohols are added, and 15 mL potassium hydroxide solutions, the vibration of side edged is added It shakes, in 85 DEG C of water bath with thermostatic control concussion saponification 30min after mixing, is cooled to room temperature immediately with cold water after saponification, saponification liquor is transferred to In 100 mL brown volumetric flasks, and conical flasks are washed with 40 mL moisture time, washing lotion is also transferred in measuring bottle, and water is added to be settled to quarter Degree, shakes up, and precision measures above-mentioned saponification liquor 2mL into 100 mL brown measuring bottles, adds 1.5 mL of hydrochloric acid solution, mixes, adds methanol It is diluted to scale, is shaken up, this solution is taken to cross 0.22 μm of organic system filter membrane, subsequent filtrate is taken to measure for high performance liquid chromatography；
C, the production of standard curve: vitamin E standard series working solution is injected separately into high performance liquid chromatograph, measures phase The peak area answered draws standard curve by abscissa of standard test liquid concentration, calculates linear regression using peak area as ordinate Equation；
D, chromatographic condition: chromatographic column C18Column；Mobile phase: methanol；Flow velocity: 0.8mL/min；Column temperature: 20 DEG C；Detection wavelength: 294 nm；Sampling volume: the test solution of step B is analyzed through high performance liquid chromatograph, measures peak area, using external standard by 10 μ L Method calculates its concentration by above-mentioned standard curve.
6. content assaying method according to claim 1-5, which is characterized in that the system of step B test solution It is standby to be operated under light protected environment.
7. content assaying method according to claim 1-5, which is characterized in that vessel used in the method Oxidizing substance must not be contained.
8. content assaying method according to claim 1-5 measurement the health care product containing vitamin E, drug or Application in food.
9. application according to claim 8, which is characterized in that the health care product is by D- α-D-α-tocopherol acetate, gelatin, pure Change water, corn oil, glycerol composition.
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