CN108645923B - Method for simultaneously determining sanshoamides and capsaicin in food - Google Patents
Method for simultaneously determining sanshoamides and capsaicin in food Download PDFInfo
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- YKPUWZUDDOIDPM-SOFGYWHQSA-N capsaicin Chemical compound COC1=CC(CNC(=O)CCCC\C=C\C(C)C)=CC=C1O YKPUWZUDDOIDPM-SOFGYWHQSA-N 0.000 title claims abstract description 140
- 229960002504 capsaicin Drugs 0.000 title claims abstract description 70
- 235000017663 capsaicin Nutrition 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 33
- 235000013305 food Nutrition 0.000 title claims abstract description 31
- 239000000523 sample Substances 0.000 claims abstract description 56
- 239000012224 working solution Substances 0.000 claims abstract description 30
- 108010068370 Glutens Proteins 0.000 claims abstract description 15
- 235000021312 gluten Nutrition 0.000 claims abstract description 15
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 7
- 241000032846 Zanthoxylum bungeanum Species 0.000 claims abstract 2
- 238000004458 analytical method Methods 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 132
- XJQPQKLURWNAAH-UHFFFAOYSA-N dihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCCC(C)C)=CC=C1O XJQPQKLURWNAAH-UHFFFAOYSA-N 0.000 claims description 49
- RBCYRZPENADQGZ-UHFFFAOYSA-N dihydrocapsaicin Natural products COC1=CC(COC(=O)CCCCCCC(C)C)=CC=C1O RBCYRZPENADQGZ-UHFFFAOYSA-N 0.000 claims description 49
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 claims description 44
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 36
- 241000949456 Zanthoxylum Species 0.000 claims description 36
- 239000000706 filtrate Substances 0.000 claims description 30
- 239000011550 stock solution Substances 0.000 claims description 30
- KWGRBVOPPLSCSI-UHFFFAOYSA-N d-ephedrine Natural products CNC(C)C(O)C1=CC=CC=C1 KWGRBVOPPLSCSI-UHFFFAOYSA-N 0.000 claims description 22
- 229960002179 ephedrine Drugs 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 15
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- 238000002156 mixing Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 238000005259 measurement Methods 0.000 claims description 10
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- 239000000126 substance Substances 0.000 claims description 8
- 230000003252 repetitive effect Effects 0.000 claims description 7
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 101000610640 Homo sapiens U4/U6 small nuclear ribonucleoprotein Prp3 Proteins 0.000 claims description 5
- 101001110823 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) 60S ribosomal protein L6-A Proteins 0.000 claims description 5
- 101000712176 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) 60S ribosomal protein L6-B Proteins 0.000 claims description 5
- 102100040374 U4/U6 small nuclear ribonucleoprotein Prp3 Human genes 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000012487 rinsing solution Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000012491 analyte Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 abstract description 7
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 12
- 235000002566 Capsicum Nutrition 0.000 description 10
- 239000006002 Pepper Substances 0.000 description 9
- 241000722363 Piper Species 0.000 description 9
- 235000016761 Piper aduncum Nutrition 0.000 description 9
- 235000017804 Piper guineense Nutrition 0.000 description 9
- 235000008184 Piper nigrum Nutrition 0.000 description 9
- 244000089698 Zanthoxylum simulans Species 0.000 description 8
- 239000000047 product Substances 0.000 description 8
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- 238000002372 labelling Methods 0.000 description 5
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- FBUBVLUPUDBFME-UHFFFAOYSA-N Xanthoxylin Chemical compound COC1=CC(O)=C(C(C)=O)C(OC)=C1 FBUBVLUPUDBFME-UHFFFAOYSA-N 0.000 description 4
- 235000021259 spicy food Nutrition 0.000 description 4
- 240000008574 Capsicum frutescens Species 0.000 description 2
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- 238000009776 industrial production Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
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- 241000251468 Actinopterygii Species 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001408 amides Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001390 capsicum minimum Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
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- 235000013312 flour Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a method for simultaneously determining sanshoamides and capsaicin in food, which comprises the following steps: 1) preparation of mixed standard working solution, 2) instrument configuration, 3) drawing of a standard curve, 4) sample preparation, 5) sample solution preparation, 6) volume fixing, 7) chromatographic analysis, 8) result analysis. The method for simultaneously measuring the zanthoxylum bungeanum and the capsaicin in the food has the characteristics of simplicity, convenience, rapidness, good accuracy and high sensitivity, effectively solves the problem of monitoring the tingling and the hot sense of terminal products such as spicy gluten food and the like, and has practical application value.
Description
Technical Field
The invention relates to a determination method, in particular to a method for simultaneously determining sanshoamides and capsaicin in food.
Background
With the development of society, spicy food is more and more popular with people, especially in Hunan, Sichuan and other places, the sales of spicy gluten food is also increased year by year, and in the production of spicy gluten food, the essential seasonings are hot pepper and Chinese prickly ash or products thereof.
In industrial production, before raw materials are selected, capsaicin and zanthoxylum or zanthoxylum oil in products of the capsaicin and the zanthoxylum are respectively measured, but after the materials are mixed in the later period, the chili powder and the Chinese prickly ash powder or the zanthoxylum oil are mixed and scattered on the surface of gluten, the content of the capsaicin and the zanthoxylum oil cannot be measured simultaneously by the existing measuring method, the zanthoxylum oil and the capsaicin cannot be separated by the existing measuring method, and therefore, in the existing industrial production, the quality monitoring of the front end of the gluten food can only be realized, and the monitoring of the terminal products of the gluten food cannot be realized.
Disclosure of Invention
The invention aims to provide a method for simultaneously measuring xanthoxylin and capsaicin in food, which has the characteristics of simplicity, convenience, rapidness, good accuracy and high sensitivity, effectively solves the problem of monitoring the tingling and the hot feeling of terminal products such as spicy gluten food and the like, and has practical application value.
In order to realize the purpose, the invention adopts the technical scheme that: a method for simultaneously measuring sanshoamides and capsaicin in food comprises the following steps:
1) preparing a mixed standard working solution;
2) configuring an instrument;
3) drawing a standard curve;
4) and (3) sample preparation: taking 2-5g of the uniformly crushed sample, adding 18-20mL of methanol into a centrifuge tube, carrying out vortex for 1-2min, carrying out ultrasonic extraction for 25-35min, centrifuging for 5-7min by using a centrifuge at the rotation speed of 4000 plus materials of 5000r/min, filtering, and transferring the filtrate to a 50mL volumetric flask;
5) and preparing a sample solution: adding 18-20mL of methanol into the filter residue obtained in the step 4), sequentially performing vortex extraction, ultrasonic extraction, centrifugation and filtration to obtain a filtrate, transferring the filtrate into the volumetric flask obtained in the step 2), and combining the filtrate with the filtrate obtained in the step 4);
6) and constant volume: rinsing the residue filtered in the step 5) with 4-6mL of methanol for 2-3 times, introducing the rinsing solution into the volumetric flask in the step 2), shaking up, metering the volume to 50mL with methanol, mixing uniformly, and filtering with a 0.22-micron organic microporous filter membrane;
7) and chromatographic analysis: carrying out chromatographic analysis on the filtrate filtered by the 0.22 mu m organic microporous filter membrane in the step 6);
8) and analyzing results.
Preferably, the step 4), sample preparation, finished spicy gluten food and the like are used as the determination sample.
Preferably, the step 1) and the preparation of the mixed standard working solution comprise the following steps:
(1) standard stock solutions: accurately weighing appropriate amount of capsaicin and dihydrocapsaicin (accurate to 0.0001 g), diluting to constant volume with methanol, preparing standard stock solutions of capsaicin and dihydrocapsaicin with concentration of 1000mg/L, storing in refrigerator at 4 deg.C, and prolonging effective period for 1 year;
(2) mixing standard stock solutions: accurately sucking appropriate amount of capsaicin and dihydrocapsaicin respectively into a 10mL volumetric flask, and diluting to the constant volume with methanol to prepare capsaicin and dihydrocapsaicin mixed standard stock solutions with contents of 200mg/L and 100mg/L respectively; storing in refrigerator at 4 deg.C for 1 year;
(3) mixing standard working solution: accurately sucking various volumes of zanthoxylum bungeanum Maxim standard stock solution (methanol solution of 100 mug/mL, university in southwest) and capsaicin and dihydrocapsaicin mixed standard stock solution respectively, dissolving with methanol and fixing the volume to prepare a series of standard working solutions; storing at below-20 deg.C for 6 months.
Preferably, the step 2) and the apparatus configuration comprise: high performance liquid chromatograph, ultraviolet detector, electronic balance, tissue triturator, vortex mixer, ultrasonic cleaner, centrifuge tube, 50mL volumetric flask, and 0.22 μm organic microporous filter membrane.
Preferably, in the step 3) and the step 7), the chromatographic conditions are as follows:
a chromatographic column: RP18 column, 5 μm, 4.6X 250mm or equivalent chromatography column;
mobile phase: acetonitrile-water, the volume percentage of acetonitrile is 40-50%;
flow rate: 0.8-1.2 mL/min;
measuring wavelength: 205-280 nm;
sample introduction amount: 5-20 μ L; column temperature: 30-40 ℃;
needle washing solvent: acetonitrile-water, the volume percentage of acetonitrile is 40-50%;
sealing the cleaning solution: 10% -30% methanol or acetonitrile water solution.
Preferably, the step 3) and the standard curve are drawn as follows: and respectively injecting 5-20 mu L of the mixed standard working solution into a high performance liquid chromatograph, measuring corresponding peak areas, and drawing a standard curve by taking the concentration of the mixed standard working solution as a horizontal coordinate and the peak area as a vertical coordinate.
Preferably, 8) and analyzing results, wherein the content of the sanshoamides in the sample is calculated according to the formula (i);
in the formula:
c, the content of the component to be detected in the sample is gram per kilogram;
C1、C2、C3the concentration of the substance to be detected in the sample liquid is obtained from the standard curve, and the unit is milligram per liter;
f1、f2、f3the conversion coefficients of the zanthoxylum ephedrine corresponding to the zanthoxylum ephedrine peak 1, the zanthoxylum ephedrine peak 2 and the zanthoxylum ephedrine peak 3 are obtained by the test result of the zanthoxylum ephedrine standard solution, and the ratio of the zanthoxylum ephedrine peak 1, the zanthoxylum ephedrine peak 2 and the zanthoxylum ephedrine peak 3 to the sum of the peak areas of the 3 peaks is obtained;
v is the volume of the sample with constant volume, and the unit is milliliter;
m is the sample mass in grams;
the calculation result is represented by the arithmetic mean value of two independent measurement results obtained under the repetitive condition, and the result retains three significant digits;
calculating the content of capsaicin and dihydrocapsaicin in the sample according to the formula II;
in the formula:
c, the content of the component to be detected in the sample is gram per kilogram;
C0-the concentration of the analyte in the sample fluid, in milligrams per liter, is determined from the standard curve;
v is the volume of the sample with constant volume, and the unit is milliliter;
m is the sample mass in grams;
the calculation results are expressed as the arithmetic mean of two independent measurements obtained under repetitive conditions, with the results remaining in three significant digits.
The spicy substances in the pepper are mainly capsaicin substances, the main active ingredients are capsaicin and dihydrocapsaicin, and the content of the capsaicin and the dihydrocapsaicin directly influences the spicy degree of the pepper and pepper products. The main numb component in the pepper is an amide substance, namely zanthoxylum ephedrine (3 peaks in the chromatographic separation of a zanthoxylum ephedrine reference substance are respectively expressed by zanthoxylum ephedrine 1, zanthoxylum ephedrine 2 and zanthoxylum ephedrine 3), and the content of the zanthoxylum ephedrine and the numb degree of the zanthoxylum bungeanum product are directly influenced. In the processing and production process of spicy foods such as gluten, capsaicin and dihydrocapsaicin are mainly reflected in the spicy sense of the spicy foods; the zanthoxylum numb essence is the numb feeling of spicy food. The total content of capsaicin in the capsicum is the sum of the contents of capsaicin and dihydrocapsaicin, and the content of sanshoamides is the sum of the contents of sanshoamides 1, 2 and 3.
The invention has the beneficial effects that: (1) the invention provides a method for ultrasonically extracting sanshoamides, capsaicin and dihydrocapsaicin by using methanol as an extraction solvent and separating and measuring the sanshoamides, the capsaicin and the dihydrocapsaicin by adopting a high performance liquid chromatography.
(2) The xanthoxylin, capsaicin and dihydrocapsaicin respectively have good linearity in the ranges of the concentration of 1-50mg/L, 2-100mg/L and 1-50mg/L, and the correlation coefficients are all larger than 0.995; the qualitative detection limits of the sanshoamides, capsaicin and dihydrocapsaicin are respectively 0.05mg/L, 0.1mg/L and 0.05mg/L, and the quantitative detection limits of the tests are respectively 1.0mg/kg, 2.0mg/kg and 1.0 mg/kg; the standard recovery ranges of the zanthoxylum, the capsaicin and the dihydrocapsaicin at the low and medium concentration levels of the sample determination are 82.5 to 100.5 percent, 93.7 to 114.8 percent and 81.1 to 110.7 percent respectively.
(3) The method has the characteristics of simplicity, convenience, rapidness, good accuracy, high sensitivity and the like, and the acetonitrile is used as the specific mobile phase, so that the problem of spicy and hot feeling monitoring of terminal products such as spicy gluten food and the like is effectively solved, and the method has practical application value.
Drawings
FIG. 1 is a chromatogram of a standard working solution mixed by sanshoamides, capsaicin and dihydrocapsaicin. (rotated 90 degrees counterclockwise)
FIG. 2 is a chromatogram of a gluten sample according to the invention. (rotated 90 degrees counterclockwise)
The text labels in the figures are represented as: 1.1, 1 of sanshoamides; 2. 2, Chinese prickly ash numb element; 3.3, zanthoxylum tingle and numb element; 4. capsaicin; 5. dihydrocapsaicin.
Detailed Description
The present invention is described in detail below for the purpose of better understanding technical solutions of the present invention by those skilled in the art, and the description of the present invention is only exemplary and explanatory and should not be construed as limiting the scope of the present invention in any way.
The following are specific examples
Example 1
A method for simultaneously measuring sanshoamides and capsaicin in food comprises the following steps:
1) and preparing a mixed standard working solution:
(1) standard stock solutions: accurately weighing appropriate amount of capsaicin (97.5%, China institute for food and drug testing), and dihydrocapsaicin standard (98.5%, China institute for food and drug testing), metering volume with methanol, and preparing standard stock solutions of capsaicin and dihydrocapsaicin with concentration of 1000 mg/L; storing in refrigerator at 4 deg.C for 1 year;
(2) mixing standard stock solutions: accurately sucking appropriate amount of capsaicin and dihydrocapsaicin respectively into a 10mL volumetric flask, and diluting to the constant volume with methanol to prepare capsaicin and dihydrocapsaicin mixed standard stock solutions with contents of 200mg/L and 100mg/L respectively; storing in refrigerator at 4 deg.C for 1 year;
(3) mixing standard working solution: accurately sucking various volumes of zanthoxylum bungeanum Maxim standard stock solution (100 microgram/mL methanol solution, university of southwest) and capsaicin and dihydrocapsaicin mixed standard stock solution respectively, dissolving with methanol and fixing the volume, and preparing a series of standard working solutions according to the table 1 or other appropriate concentrations; storing at below-20 deg.C for 6 months.
2) And equipment configuration: high performance liquid chromatograph, ultraviolet detector, electronic balance, tissue triturator, vortex mixer, ultrasonic cleaner, centrifuge tube, 50mL volumetric flask, and 0.22 μm organic microporous filter membrane.
3) Drawing a standard curve:
the chromatographic conditions were as follows:
a chromatographic column: RP18 column, 5 μm, 4.6X 250mm or equivalent chromatography column;
mobile phase: acetonitrile: water =40:60 (volume fraction);
flow rate: 0.8 mL/min;
measuring wavelength: 205 nm;
sample introduction amount: 5 mu L of the solution; column temperature: 30 ℃;
needle washing solvent: acetonitrile: water =40:60 (volume fraction);
sealing the cleaning solution: 10% by volume methanol solution.
And respectively injecting 5 mu L of mixed standard working solution into a high performance liquid chromatograph, measuring corresponding peak areas under the chromatographic conditions, and drawing a standard curve by taking the concentration of the mixed standard working solution as a horizontal coordinate and the peak area as a vertical coordinate.
4) And (3) sample preparation: taking 2g of the uniformly crushed sample, adding 18mL of methanol into a centrifuge tube, carrying out vortex for 1min, carrying out ultrasonic extraction for 25min, then centrifuging for 5min by using a centrifuge at the rotation speed of 4000r/min, filtering, and transferring the filtrate to a 50mL volumetric flask;
5) and preparing a sample solution: adding 18mL of methanol into the filter residue obtained in the step 4), sequentially performing vortex extraction, ultrasonic extraction, centrifugation and filtration to obtain a filtrate, transferring the filtrate into the volumetric flask obtained in the step 2), and combining the filtrate with the filtrate obtained in the step 4);
6) and constant volume: rinsing the residue filtered in the step 5) with 4mL of methanol for 2 times, introducing the rinsing solution into the volumetric flask in the step 2), shaking up, metering the volume to 50mL with methanol, mixing uniformly, and filtering with a 0.22-micrometer organic microporous filter membrane;
7) and chromatographic analysis: carrying out chromatographic analysis on the filtrate filtered by the 0.22 mu m organic microporous filter membrane in the step 6); step 7) chromatographic conditions were the same as in step 3).
8) And analyzing results: the content of sanshoamides in the sample is calculated according to the formula I;
in the formula:
c, the content of the component to be detected in the sample is gram per kilogram (g/kg);
C1、C2、C3the concentration of the substances to be detected (sanshoamides peaks 1, 2 and 3) in the sample liquid obtained from the standard curve is milligram per liter (mg/L);
f1、f2、f3the conversion coefficients of sanshoamides corresponding to sanshoamides peak 1, peak 2 and peak 3 (the ratio of the peak areas of sanshoamides peak 1, peak 2 and peak 3 in the total of 3 peaks is obtained from the test result of sanshoamides standard solution);
v-sample volume to volume in milliliters (mL);
m is the sample mass in grams (g);
the calculation result is represented by the arithmetic mean value of two independent measurement results obtained under the repetitive condition, and the result retains three significant digits;
calculating the content of capsaicin and dihydrocapsaicin in the sample according to the formula II;
in the formula:
c, the content of the component to be detected in the sample is gram per kilogram (g/kg);
C0-the concentration of the test substance in milligram per liter (mg/L) in the sample solution is derived from the standard curve;
v-sample volume to volume in milliliters (mL);
m is the sample mass in grams (g).
The calculation results are expressed as the arithmetic mean of two independent measurements obtained under repetitive conditions, with the results remaining in three significant digits.
Example 2
A method for simultaneously measuring sanshoamides and capsaicin in food comprises the following steps:
1) and preparing a mixed standard working solution:
(1) standard stock solutions: accurately weighing appropriate amount of capsaicin (97.5%, China institute for food and drug testing), and dihydrocapsaicin standard (98.5%, China institute for food and drug testing), metering volume with methanol, and preparing standard stock solutions of capsaicin and dihydrocapsaicin with concentration of 1000 mg/L; storing in refrigerator at 4 deg.C for 1 year;
(2) mixing standard stock solutions: accurately sucking appropriate amount of capsaicin and dihydrocapsaicin respectively into a 10mL volumetric flask, and diluting to the constant volume with methanol to prepare capsaicin and dihydrocapsaicin mixed standard stock solutions with contents of 200mg/L and 100mg/L respectively; storing in refrigerator at 4 deg.C for 1 year;
(3) mixing standard working solution: accurately sucking various volumes of zanthoxylum bungeanum Maxim standard stock solution (100 microgram/mL methanol solution, university of southwest) and capsaicin and dihydrocapsaicin mixed standard stock solution respectively, dissolving with methanol and fixing the volume, and preparing a series of standard working solutions according to the table 1 or other appropriate concentrations; storing at below-20 deg.C for 6 months.
2) And equipment configuration: high performance liquid chromatograph, ultraviolet detector, electronic balance, tissue triturator, vortex mixer, ultrasonic cleaner, centrifuge tube, 50mL volumetric flask, and 0.22 μm organic microporous filter membrane.
3) Drawing a standard curve:
the chromatographic conditions were as follows:
a chromatographic column: RP18 column, 5 μm, 4.6X 250mm or equivalent chromatography column;
mobile phase: acetonitrile: water =50:50 (volume fraction);
flow rate: 1.2 mL/min;
measuring wavelength: 280 nm;
sample introduction amount: 20 mu L of the solution; column temperature: 40 ℃;
needle washing solvent: acetonitrile: water =50:50 (volume fraction);
sealing the cleaning solution: a 20% by volume aqueous acetonitrile solution.
And respectively injecting 20 mu L of mixed standard working solution into a high performance liquid chromatograph, measuring corresponding peak areas under the chromatographic conditions, and drawing a standard curve by taking the concentration of the mixed standard working solution as a horizontal coordinate and the peak area as a vertical coordinate.
4) And (3) sample preparation: taking 4g of uniformly crushed gluten sample into a centrifuge tube, adding 19mL of methanol, carrying out vortex for 2min, carrying out ultrasonic extraction for 35min, then centrifuging for 7min by using a centrifuge, carrying out filtration at the centrifuge rotation speed of 5000r/min, and transferring the filtrate to a 50mL volumetric flask;
5) and preparing a sample solution: adding 19mL of methanol into the filter residue obtained in the step 4), sequentially performing vortex extraction, ultrasonic extraction, centrifugation and filtration to obtain a filtrate, transferring the filtrate into the volumetric flask obtained in the step 2), and combining the filtrate with the filtrate obtained in the step 4);
6) and constant volume: rinsing the residue filtered in the step 5) with 6mL of methanol for 3 times, introducing the rinsing solution into the volumetric flask in the step 2), shaking up, metering the volume to 50mL with methanol, mixing uniformly, and filtering with a 0.22-micrometer organic microporous filter membrane;
7) and chromatographic analysis: carrying out chromatographic analysis on the filtrate filtered by the 0.22 mu m organic microporous filter membrane in the step 6); step 7) chromatographic conditions were the same as in step 3).
8) And analyzing results: the same as in example 1.
Example 3
A method for simultaneously measuring sanshoamides and capsaicin in food comprises the following steps:
1) and preparing a mixed standard working solution:
(1) standard stock solutions: accurately weighing appropriate amount of capsaicin (97.5%, China institute for food and drug testing), and dihydrocapsaicin standard (98.5%, China institute for food and drug testing), metering volume with methanol, and preparing standard stock solutions of capsaicin and dihydrocapsaicin with concentration of 1000 mg/L; storing in refrigerator at 4 deg.C for 1 year;
(2) mixing standard stock solutions: accurately sucking appropriate amount of capsaicin and dihydrocapsaicin respectively into a 10mL volumetric flask, and diluting to the constant volume with methanol to prepare capsaicin and dihydrocapsaicin mixed standard stock solutions with contents of 200mg/L and 100mg/L respectively; storing in refrigerator at 4 deg.C for 1 year;
(3) mixing standard working solution: accurately sucking various volumes of zanthoxylum bungeanum Maxim standard stock solution (100 microgram/mL methanol solution, university of southwest) and capsaicin and dihydrocapsaicin mixed standard stock solution respectively, dissolving with methanol and fixing the volume, and preparing a series of standard working solutions according to the table 1 or other appropriate concentrations; storing at below-20 deg.C for 6 months.
2) And equipment configuration: high performance liquid chromatograph, ultraviolet detector, electronic balance, tissue triturator, vortex mixer, ultrasonic cleaner, centrifuge tube, 50mL volumetric flask, and 0.22 μm organic microporous filter membrane.
3) Drawing a standard curve:
the chromatographic conditions were as follows:
a chromatographic column: RP18 column, 5 μm, 4.6X 250 mm;
mobile phase: acetonitrile: water =45:55 (volume fraction);
flow rate: 1.0 mL/min;
measuring wavelength: sanshoamides 268nm, capsaicin and dihydrocapsaicin 230 nm;
sample introduction amount: 10 mu L of the solution; column temperature: 35 ℃;
needle washing solvent: acetonitrile: water =45:55 (volume fraction);
sealing the cleaning solution: 20% by volume of aqueous methanol.
Respectively injecting 10 mu L of mixed standard working solution into a high performance liquid chromatograph, measuring corresponding peak areas under the chromatographic conditions, drawing a standard curve by taking the concentration of the mixed standard working solution as a horizontal coordinate and the peak area as a vertical coordinate, and taking a table 2 as a standard working solution curve equation:
as can be seen from Table 2, sanshoamides, capsaicin and dihydrocapsaicin are in linear relation with response values within the ranges of 1-50mg/L, 2-100mg/L and 1-50mg/L, and the correlation coefficient R is more than or equal to 0.995.
4) And (3) sample preparation: taking 5g of the uniformly crushed sample, adding 20mL of methanol into a centrifuge tube, carrying out vortex for 1min, carrying out ultrasonic extraction for 30min, then centrifuging for 5min by using a centrifuge at the rotation speed of 4000r/min, filtering, and transferring the filtrate to a 50mL volumetric flask;
5) and preparing a sample solution: adding 20mL of methanol into the filter residue obtained in the step 4), sequentially performing vortex extraction, ultrasonic extraction, centrifugation and filtration to obtain a filtrate, transferring the filtrate into the volumetric flask obtained in the step 2), and combining the filtrate with the filtrate obtained in the step 4);
6) and constant volume: rinsing the residue filtered in the step 5) with 5mL of methanol for 2 times, introducing the rinsing solution into the volumetric flask in the step 2), shaking up, metering the volume to 50mL with methanol, mixing uniformly, and filtering with a 0.22-micrometer organic microporous filter membrane;
7) and chromatographic analysis: carrying out chromatographic analysis on the filtrate filtered by the 0.22 mu m organic microporous filter membrane in the step 6); step 7) chromatographic conditions were the same as in step 3).
8) And analyzing results: the same as in example 1.
The following are the experimental data of the present invention:
taking example 3 as an example:
1. precision: the arithmetic mean of the two measurements was taken as the measurement result. The absolute difference between the two measurements obtained under repetitive conditions must not exceed 10% of the arithmetic mean.
2. Quantitative detection limit: when the sampling is 5g and the constant volume is 50mL, the quantitative detection limits of the sanshoamides, the capsaicin and the dihydrocapsaicin are 1.0mg/kg, 2.0mg/kg and 1.0mg/kg respectively.
3. And (3) experimental verification:
3.1 precision test
The standard solutions prepared at 1.0/2.0/1.0mg/L and 20.0/40.0/20.0mg/L were tested repeatedly for 7 times for evaluation of instrument accuracy and repeatability, and the results were as follows:
as can be seen from Table 3, the difference and RSD were both less than 10%, indicating good precision of the instrument.
3.2 repeatability test
6 parts of imperial crown gluten 1224W sample and 4 parts of self-made test sample are prepared in parallel, the determination is carried out according to the determination method, the accuracy and the repeatability of the method are evaluated, and the results are as follows: (unit: g/kg, AVE: mean, S: standard deviation, RSD: relative standard deviation).
As can be seen from Table 4, the RSD was less than 10%, indicating good reproducibility of the method.
3.3 detection limit, Linear Range, quantitative Limit
Testing the instrument detection limit: preparing 0.05/0.1/0.05mg/L standard solution, performing detection limit test for 7 times continuously, wherein the difference and RSD are less than 10 percent, and the results are as follows in the following table 5:
testing the detection limit of the method: taking 3.14 times of standard deviation of 7 repeated tests of the method blank as a method detection limit (MDL = 3.14S), estimating a concentration value according to the obtained MDL, preparing the method blank, adding a standard of 0.1/0.2/0.1mg/L, repeatedly testing for 7 times, wherein the average recovery rate is between 90 and 110 percent, and the results are as follows:
linear range test:
the detection limits of the zanthoxylum, capsaicin and dihydrocapsaicin testing instruments are 0.05mg/L, 0.1mg/L and 0.05mg/L, the detection limits of the zanthoxylum, capsaicin and dihydrocapsaicin testing methods are 0.1mg/L, 0.2mg/L and 0.1mg/L (when the sampling is 5.0g and the constant volume is 50mL, the corresponding quantitative detection limits of the zanthoxylum, capsaicin and dihydrocapsaicin are respectively 1.0mg/kg, 2.0mg/kg and 1.0 mg/kg), and the linear ranges of the zanthoxylum, capsaicin and dihydrocapsaicin are respectively 0.1 mg/L-100 mg/L, 0.2 mg/L-500 mg/L and 0.1 mg/L-250 mg/L.
3.4 standard recovery test
Selecting finished products of imperial crown gluten and spicy fish of Hunan Yufeng food company, performing sample labeling tests at low and medium concentration level points of sample determination for 2 times, performing the tests 2 times after monitoring labeling, and performing the tests 2 times after substrate labeling, wherein the results are shown in the following tables 5-6:
a semi-finished product flour embryo of Yufeng food industry Co Ltd is selected, a certain amount of ingredients are added, a test sample is prepared, and because the pepper oil and the pepper are known in amount, theoretical addition amount and recovery rate of the capsaicin, the dihydrocapsaicin and the sanshoamides can be calculated according to the amount of the pepper and the pepper oil in the ingredients and the content of the capsaicin, the dihydrocapsaicin and the sanshoamides in the pepper oil.
As can be seen from the above tables 5-7, the recovery rates of the monitoring labeling of zanthoxylum, capsaicin and dihydrocapsaicin and the substrate labeling are all 80-120%, which shows that the method and the apparatus have better accuracy and can meet the test requirements.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (4)
1. A method for simultaneously determining sanshoamides and capsaicin in food is characterized by comprising the following steps:
1) preparing a mixed standard working solution;
the step 1) and the preparation of the mixed standard working solution comprise the following steps:
(1) standard stock solutions: accurately weighing capsaicin and dihydrocapsaicin standard substances respectively, adding methanol to a constant volume to prepare capsaicin and dihydrocapsaicin standard stock solutions with the concentration of 1000mg/L, and storing in a refrigerator at 4 ℃ for 1 year;
(2) mixing standard stock solutions: accurately sucking standard capsaicin and dihydrocapsaicin respectively into a 10mL volumetric flask, and diluting to the constant volume by using methanol to prepare mixed standard capsaicin and dihydrocapsaicin stock solutions with the contents of 200mg/L and 100mg/L respectively; storing in refrigerator at 4 deg.C for 1 year;
(3) mixing standard working solution: accurately absorbing the zanthoxylum bungeanum maxim standard stock solution and the capsaicin and dihydrocapsaicin mixed standard stock solution with different volumes respectively, dissolving by using methanol, and fixing the volume to prepare a series of standard working solutions; storing at below-20 deg.C for 6 months;
2) configuring an instrument;
the step 2) and the equipment configuration comprise: a high performance liquid chromatograph, an ultraviolet detector, an electronic balance, a tissue triturator, a vortex mixer, an ultrasonic cleaner, a centrifuge tube, a 50mL volumetric flask and a 0.22 μm organic microporous filter membrane;
3) drawing a standard curve;
4) and (3) sample preparation: taking 2-5g of the uniformly crushed sample, adding 18-20mL of methanol into a centrifuge tube, carrying out vortex for 1-2min, carrying out ultrasonic extraction for 25-35min, centrifuging for 5-7min by using a centrifuge at the rotation speed of 4000 plus materials of 5000r/min, filtering, and transferring the filtrate to a 50mL volumetric flask;
5) and preparing a sample solution: adding 18-20mL of methanol into the filter residue obtained in the step 4), sequentially performing vortex extraction, ultrasonic extraction, centrifugation and filtration to obtain a filtrate, transferring the filtrate into the volumetric flask obtained in the step 2), and combining the filtrate with the filtrate obtained in the step 4);
6) and constant volume: rinsing the residue filtered in the step 5) with 4-6mL of methanol for 2-3 times, introducing the rinsing solution into the volumetric flask in the step 2), shaking up, metering the volume to 50mL with methanol, mixing uniformly, and filtering with a 0.22-micron organic microporous filter membrane;
7) and chromatographic analysis: carrying out chromatographic analysis on the filtrate filtered by the 0.22 mu m organic microporous filter membrane in the step 6);
8) and analyzing results;
wherein, in the step 3) and the step 7), the chromatographic conditions are as follows:
a chromatographic column: RP18 column, 5 μm, 4.6X 250 mm;
mobile phase: acetonitrile-water, the volume percentage of acetonitrile is 40-50%;
flow rate: 0.8-1.2 mL/min;
measuring wavelength: 205-280 nm;
sample introduction amount: 5-20 μ L; column temperature: 30-40 ℃;
needle washing solvent: acetonitrile-water, the volume percentage of acetonitrile is 40-50%;
sealing the cleaning solution: 10% -30% methanol or acetonitrile water solution.
2. The method for simultaneously measuring sanshoamides and capsaicin in food according to claim 1, wherein the step 4) and the sample preparation comprise finished spicy gluten food as the measurement sample.
3. The method for simultaneously determining sanshoamides and capsaicin in food according to claim 1, wherein the standard curve of 3) and the standard curve of capsaicin are drawn as follows: and respectively injecting 5-20 mu L of the mixed standard working solution into a high performance liquid chromatograph, measuring corresponding peak areas, and drawing a standard curve by taking the concentration of the mixed standard working solution as a horizontal coordinate and the peak area as a vertical coordinate.
4. The method for simultaneously determining sanshoamides and capsaicin in food according to claim 1, wherein the 8) result analysis is carried out, and the content of the sanshoamides in a sample is calculated according to the formula (I);
in the formula:
c, the content of the component to be detected in the sample is gram per kilogram;
C1、C2、C3the concentration of the substance to be detected in the sample liquid is obtained from the standard curve, and the unit is milligram per liter;
f1、f2、f3the conversion coefficients of the zanthoxylum ephedrine corresponding to the zanthoxylum ephedrine peak 1, the zanthoxylum ephedrine peak 2 and the zanthoxylum ephedrine peak 3 are obtained by the test result of the zanthoxylum ephedrine standard solution, and the ratio of the zanthoxylum ephedrine peak 1, the zanthoxylum ephedrine peak 2 and the zanthoxylum ephedrine peak 3 to the sum of the peak areas of the 3 peaks is obtained;
v is the volume of the sample with constant volume, and the unit is milliliter;
m is the sample mass in grams;
the calculation result is represented by the arithmetic mean value of two independent measurement results obtained under the repetitive condition, and the result retains three significant digits;
calculating the content of capsaicin and dihydrocapsaicin in the sample according to the formula II;
in the formula:
c, the content of the component to be detected in the sample is gram per kilogram;
C0-the concentration of the analyte in the sample fluid, in milligrams per liter, is determined from the standard curve;
v is the volume of the sample with constant volume, and the unit is milliliter;
m is the sample mass in grams;
the calculation results are expressed as the arithmetic mean of two independent measurements obtained under repetitive conditions, with the results remaining in three significant digits.
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Denomination of invention: A method for simultaneous determination of zanthoxylin and capsaicin in food Effective date of registration: 20220524 Granted publication date: 20211130 Pledgee: Hunan Pingjiang Rural Commercial Bank Co.,Ltd. Pledgor: HUNAN YUFENG FOOD INDUSTRIAL CO.,LTD. Registration number: Y2022980006126 |
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Effective date of registration: 20240523 Address after: Xingye Road, High-tech Industrial Park, Wushi Town, Pingjiang County, Yueyang City, Hunan Province 410400 Patentee after: Hunan Spicy Prince Food Co.,Ltd. Country or region after: China Address before: 414000 Pingjiang Industrial Park, Yueyang City, Hunan Province Patentee before: HUNAN YUFENG FOOD INDUSTRIAL CO.,LTD. Country or region before: China |