CN103630504A - Detection of trace copper in preserved eggs - Google Patents
Detection of trace copper in preserved eggs Download PDFInfo
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- CN103630504A CN103630504A CN201210311708.XA CN201210311708A CN103630504A CN 103630504 A CN103630504 A CN 103630504A CN 201210311708 A CN201210311708 A CN 201210311708A CN 103630504 A CN103630504 A CN 103630504A
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- sample
- copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 30
- 239000010949 copper Substances 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title abstract description 10
- 235000013601 eggs Nutrition 0.000 title abstract 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 8
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000523 sample Substances 0.000 claims description 11
- 239000012086 standard solution Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims description 2
- 239000012159 carrier gas Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910052805 deuterium Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 230000004907 flux Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000010354 integration Effects 0.000 claims description 2
- 239000012488 sample solution Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 4
- 239000003607 modifier Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004380 ashing Methods 0.000 abstract 1
- 238000000889 atomisation Methods 0.000 abstract 1
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 abstract 1
- QWARLPGIFZKIQW-UHFFFAOYSA-N hydrogen peroxide;nitric acid Chemical compound OO.O[N+]([O-])=O QWARLPGIFZKIQW-UHFFFAOYSA-N 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000002133 sample digestion Methods 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 description 4
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 238000001636 atomic emission spectroscopy Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000005375 photometry Methods 0.000 description 2
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 208000027219 Deficiency disease Diseases 0.000 description 1
- 208000002972 Hepatolenticular Degeneration Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 208000001024 intrahepatic cholestasis Diseases 0.000 description 1
- 230000007872 intrahepatic cholestasis Effects 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses detection of trace copper content in preserved eggs through graphite furnace atomic absorption spectrometry. By utilization of strong oxidizing property of a concentrated nitric acid-hydrogen peroxide system, sample digestion is carried out, and the sample is transparent faint yellow. Ammonium sulfate is employed as a matrix modifier. Optimum conditions of the concentration of the matrix modifier, ashing temperature, atomization temperature and the like are selected, and the detection of trace copper in preserved eggs is carried out under the conditions. The recovery rate is 88.9%-95.8% and the detection limit is 0.0205 micrograms/L. The method is advantaged by high accuracy, good selectivity and low detection limit, is especially suitable for detection of trace copper, and has good technology popularization values.
Description
One, technical field
The invention belongs to physical and chemical inspection technical field, be specifically related to the detection method of copper trace in lime-preserved egg.
Two, background technology
Fresh smooth mouthful of lime-preserved egg mouthfeel, color, smell and taste all have one's own knack.In the traditional lime-preserved egg processing formula of China, all added massicot (yellow lead powder), make aobvious beautiful preserved egg on lime-preserved egg albumen.Because lead is a kind of heavy metal element of poisonous savings, a lot of countries make and prohibit pin life it, and this impact of market on lime-preserved egg is very large.Pickling of lime-preserved egg improved technique now, with copper sulphate, zinc etc., replaces massicot, do not use lead compound, and " lead-free preserved egg " gains the name thus.The synthetic aspect of copper to painted, the collagen of the growth of bone, hair, plays an important role.Copper is distributed in each position of the person, and lacking copper is to cause deficiency disease, excessively may cause again poisoningly, comprises the illnesss such as acute copper poisoning, hepatolenticular degeneration, children's intrahepatic cholestasis.Therefore China's food standard has also been stipulated strict limiting the quantity of to copper.
The detection method of copper mainly contains inductively coupled plasma one atomic emission spectrometry (ICP-AES), micro-wave digestion one Solid-Phase Extraction photometry, atomic absorption spectrography (AAS) etc.Photometry method is simple, quick, but sensitivity is lower, is commonly used for microanalysis, still immature for the trace level analysis in food or biosome.Inductively coupled plasma one atomic emission spectrometry (ICP-AES) method is that trace element is analysed state-of-the-art method in field, can be used for the mensuration of the removal of mercury most heavy metals in addition, but it is expensive, vulnerable to pollution.In using mineral carbon stove aas determination egg products, copper trace has no report, and the present invention selects graphite oven atomic absorption, and by condition determination is optimized, its precision, accuracy improve greatly, and the batch of applicable copper trace is measured.
Three, summary of the invention
The present invention includes two key steps:
1, lime-preserved egg sample is cleared up preparation liquid to be measured through red fuming nitric acid (RFNA)-hydrogen peroxide system.
2, with ammonium sulfate, make matrix modifier, adopt graphite oven atomic absorption, deuterium lamp correcting background, according to the content of copper in standard curve determination liquid to be measured.
Four, embodiment
Determining of embodiment 1 typical curve
1, main agents and instrument
1g/L copper standard solution (accurately take and analyze pure elemental copper 0.1000g, dissolve with red fuming nitric acid (RFNA), accurately prepare 100ml); 1mg/L copper standard solution (accurately get 0.10ml copper standard reserving solution, be diluted to 100ml with nitric acid); Red fuming nitric acid (RFNA) (top grade is pure, Urumchi chemical reagent factory); 30% hydrogen peroxide (top grade is pure, Xi'an chemical reagent factory); Ammonium sulfate (top grade is pure, Xi'an chemical reagent factory)
AAS7000 atomic absorption spectrophotometer (AAS) (Japanese Shimadzu), is equipped with graphite-pipe, copper hollow cathode lamp; HR2000 electronic analytical balance (sensibility reciprocal 0.0001g, Shanghai Hengping Science Instrument Co., Ltd.)
2, instrument condition of work
Detect wavelength: 324.8nm; Slit: 0.5nm; Lamp current: 6mA; Carrier gas flux (Ar): 200mL/min; Sample size: 20 μ L; Mensuration mode: peak area integration
Table 1 graphite furnace heating schedule
3, typical curve
It is 2.5,5.0,7.5,10.0 that nitric acid with 0.4% becomes concentration by 1mg/L copper standard solution stepwise dilution, 12.5,15.0,17.5,20.0, and the standard solution of 25.0 μ g/L.0.4% nitric acid is done blank, and in standard solution and blank solution, the concentration of matrix modifier ammonium sulfate is 1%.With drawing standard curve, obtain regression equation A=1.14286E-4+0.05429C, r=0.9994.
In formula, A---absorbance; C---concentration (μ g/L)
The mensuration of copper content in embodiment 2 lime-preserved egg
1, the mensuration of copper content in lime-preserved egg
Accurately take 5.0000g sample in clearing up bottle, add 3.30mL red fuming nitric acid (RFNA) and 2.00mL 30% hydrogen peroxide, be heated to sample solution and be faint yellow supernatant liquid, and stop smoldering.After cooling, transfer in 100mL volumetric flask, use distilled water constant volume, mix, stand-by.Get 1.0mL constant volume liquid in 50mL volumetric flask, add ammonium sulfate, 0.4% salpeter solution constant volume, to be measured, now, in solution to be measured, the concentration of ammonium sulfate is 1%.Parallelly make 7 groups of samples, do blank assay simultaneously, the content of measuring copper in lime-preserved egg according to instrument condition of work and typical curve equation is 4.404mg/Kg, and RSD is 2.4%.
2, accuracy experiment
Accurately take 5.0000g sample in clearing up bottle, add 3.30mL red fuming nitric acid (RFNA) and 2.00mL 30% hydrogen peroxide, add respectively 10.0mL copper standard solution (add scalar and be about 0.5 times of copper content in sample).With reference to " mensuration of copper content in lime-preserved egg " method, prepare liquid to be measured.Parallelly make 7 groups of samples, do blank assay simultaneously, according to instrument condition of work and typical curve equation, measure the content of copper.By the method, measure respectively again that to add scalar be 1 times, sample, the recovery in the time of 2 times, i.e. label taking liquid 20mL respectively, 40mL carries out recovery testu to sample, the results are shown in Table 2:
The recovery of table 2 copper
As shown in Table 2, the recovery is between 90.8%-94.7, and the accuracy of this method is higher.
3, the mensuration of detection limit
With reference to " mensuration of copper content in lime-preserved egg " method, prepare blank liquid to be measured.Parallelly make 20 groups of samples, take reagent blank as background, according to instrument condition of work and typical curve equation, measure the content of copper in blank sample.According to IUPAC (IUPAC), get k=3 and calculate to detect and be limited to 1.127 μ g/L.
Claims (5)
1. take 5.0000g sample in clearing up bottle, add 3.30mL red fuming nitric acid (RFNA) and 2.00mL 30% hydrogen peroxide, be heated to sample solution and be faint yellow supernatant liquid, and stop smoldering.After cooling, transfer in 100mL volumetric flask, use distilled water constant volume.
2. get 1.0mL constant volume liquid in 50mL volumetric flask, add ammonium sulfate, 0.4% salpeter solution constant volume, this solution is liquid to be measured, now, in solution to be measured, the concentration of ammonium sulfate is 1%.
3. adopt graphite oven atomic absorption, utilize deuterium lamp correcting background, according to the content of copper in standard curve determination liquid to be measured: atomic absorption analysis condition is: detect wavelength 324.8nm; Slit 0.5nm; Lamp current 6mA; Carrier gas flux 200mL/min; Sample size 20 μ L; Peak area integration is measured mode.
4. graphite furnace heating schedule is as follows:
5. accuracy experiment: accurately take 5.0000g sample in clearing up bottle, add 3.30mL red fuming nitric acid (RFNA) and 2.00mL 30% hydrogen peroxide, add respectively copper standard solution, add scalar and be about respectively 0.5 times, 1.0 times, 2.0 times of copper content in sample, clear up afterwards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210311708.XA CN103630504A (en) | 2012-08-29 | 2012-08-29 | Detection of trace copper in preserved eggs |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210311708.XA CN103630504A (en) | 2012-08-29 | 2012-08-29 | Detection of trace copper in preserved eggs |
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| Publication Number | Publication Date |
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| CN103630504A true CN103630504A (en) | 2014-03-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210311708.XA Pending CN103630504A (en) | 2012-08-29 | 2012-08-29 | Detection of trace copper in preserved eggs |
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| Country | Link |
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| CN (1) | CN103630504A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290194A (en) * | 2016-08-22 | 2017-01-04 | 常州大学 | A kind of method of cadmium content in direct mensuration electron level diethylene glycol dimethyl ether |
| CN113504190A (en) * | 2021-06-30 | 2021-10-15 | 广东环凯生物技术有限公司 | Rapid detection method and reagent for water quality trace copper |
| CN118583804A (en) * | 2024-08-06 | 2024-09-03 | 广州科技贸易职业学院 | A method for detecting copper contaminants in hemodialysis concentrate |
-
2012
- 2012-08-29 CN CN201210311708.XA patent/CN103630504A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290194A (en) * | 2016-08-22 | 2017-01-04 | 常州大学 | A kind of method of cadmium content in direct mensuration electron level diethylene glycol dimethyl ether |
| CN113504190A (en) * | 2021-06-30 | 2021-10-15 | 广东环凯生物技术有限公司 | Rapid detection method and reagent for water quality trace copper |
| CN118583804A (en) * | 2024-08-06 | 2024-09-03 | 广州科技贸易职业学院 | A method for detecting copper contaminants in hemodialysis concentrate |
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Application publication date: 20140312 |
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