CN102707002B - The method of various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce - Google Patents
The method of various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce Download PDFInfo
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Abstract
The invention discloses the method for various antiseptic content in a kind of capillary gas chromatography internal standard method Simultaneously test soy sauce, it comprises the following steps: (1) takes soy sample; (2) add internal standard substance solution in the sample to which, then carry out acidifying, extracted by ether successively, purification dewaters and concentration, obtains sample solution; (3) sample solution got in step (2) carries out gas chromatographic analysis, obtains chromatogram analysis data; (4) by the chromatogram analysis data of the acquisition of step (3) and the comparison of predetermined antiseptic normal data, the content of various antiseptic in soy sauce is obtained.The method can the content of the antiseptic such as benzoic acid, sorbic acid, dehydroactic acid and parabens in Simultaneously test soy sauce, and easy to operation, effectively can reduce the impact of the factor such as operate miss and instrument condition on measurement result, result accurately and reliably.
Description
Technical field
The present invention relates to a kind of method detecting various antiseptic content in soy sauce, the method for various antiseptic content in especially a kind of capillary gas chromatography internal standard method Simultaneously test soy sauce.
Background technology
Soy sauce is a kind of flavouring being rich in nutrition, delicious flavour, may occur putrid and deteriorated when being subject to the pollution of microorganism, therefore, manufacturer can add some food antisepticses to suppress the corruption that may be formed, and antiseptic conventional in soy sauce has benzoic acid, sorbic acid and parabens etc.The limitation of national standard to antiseptic makes explicit provisions, and within the scope of safe handling, antiseptic is to human non-toxic's spinoff, but excessive eating has certain toxicity to human body.Examination criteria relevant is at present GB/T 5009.29-2003 " in food sorbic acid, benzoic mensuration " and the GB/T 5009.31-2003 mensuration of parabens " in the food ", if directly adopt standard method to carry out the mensuration of various antiseptic content in soy sauce, a sample carries out pre-service respectively by two kinds of methods and adopts different instrument conditions, wastes time and energy.And find through practice, when directly adopting this standard to detect soy sauce series products, recovery of standard addition is lower, and measurement result is unstable, and also easily when extracting comparatively dense thick dark soy sauce class sample is difficult to layering because of the generation of emulsion and carries out subsequent operation.When therefore directly adopting the vapor-phase chromatography in this standard particularly dark soy sauce class sample detect to soy sauce series products, precision and accuracy are all not ideal enough, this is owing to adopting quantified by external standard method, it is the generation that sample preparation or instrument condition all may cause error, loaded down with trivial details determination step adds the occurrence probability of operate miss, upper machine measures requirement especially must have quite high instrument performance and configuration, such as, need configuration automatic sampler to guarantee accurately to control sample size etc.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides the method for various antiseptic content in a kind of capillary gas chromatography internal standard method Simultaneously test soy sauce, the method can the content of the antiseptic such as benzoic acid, sorbic acid, dehydroactic acid and parabens in Simultaneously test soy sauce, easy to operation, effectively can reduce the impact of the factor such as operate miss and instrument condition on measurement result, result accurately and reliably.
The object of the invention is to be realized by following technical measures: a kind of method of various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce, it comprises the following steps:
(1) soy sample is taken;
(2) add internal standard substance solution in the sample to which, then carry out acidifying, extracted by ether successively, purification dewaters and concentration, obtains sample solution;
(3) sample solution got in step (2) carries out gas chromatographic analysis, obtains chromatogram analysis data;
(4) by the correction factor comparison of the chromatogram analysis data of the acquisition of step (3) and each antiseptic to be measured, the content of various antiseptic in soy sauce is obtained.
The consumption of described soy sample can be taken according to different soy sauce classification in step of the present invention (1).As the embodiment of in the present invention, light soy sauce class soy sauce recommends the amount of taking between 0.5 ~ 2.5g scope, and dark soy sauce class soy sauce recommends the amount of taking between 0.5 ~ 1.0g scope.
During due to dark soy sauce class soy sauce employing extracted by ether, easily there is emulsification, cause reaching the object effectively extracting antiseptic, thus in step of the present invention (1) as sample be dark soy sauce class soy sauce time, pre-service need be carried out to dark soy sauce class soy sauce: add in dark soy sauce class soy sample sodium chloride solution dilution 1 ~ 2.5 times.
As one embodiment of the present invention, described step (2) uses following concrete operations: soy sample is placed in tool plug container, accurately add 0.3 ~ 0.7ml inner mark solution, add 0.3 ~ 0.7ml hydrochloric acid solution again, mixing, 2 extractions are divided with 20 ~ 40ml ether, merge twice upper solution, then in the upper solution of gained, 3 ~ 5ml sodium bisulfate is added, vibration, carry out washing, purifying, leave standstill, in upper solution, add 3 ~ 7g anhydrous sodium sulfate after removing lower floor's solution dewater, then in 40 ~ 45 DEG C of water-baths, nitrogen flushing is concentrated into 0.1 ~ 1ml, use 2 ~ 2.5ml acetone diluted again, sample solution.Add hcl acidifying in soy sample after, the antiseptic that Sodium Benzoate wherein, potassium sorbate etc. exist in a salt form is converted into organic acid, extract with ether, residual water-soluble interfering component is removed again with niter cake washing, purifying, absorb water with anhydrous sodium sulfate, be namely available on the machine and detect, simplify the pretreated process of soy sample, improve work efficiency, decrease the use of organic solvent simultaneously.
Tool plug container of the present invention can adopt tool plug graduated cylinder, tool plug test tube or color comparison tube.
The chromatographic condition that step of the present invention (3) is recommended is: described capillary chromatographic column adopts polarity capillary chromatographic column, and requirement can realize good separation to each component to be measured and internal standard compound matter simultaneously; Constant temperature or suitable temperature programme; Constant current or constant voltage, manually or automatically sample introduction 0.5 ~ 1.0 μ l, carrier gas is high pure nitrogen, column cap pressure 0.05 ~ 1Mpa, split ratio 50 ~ 100 ﹕ 1.
The column temperature of described constant temperature about 200 ~ 220 DEG C.
Described temperature programme condition is: initial temperature 120 ~ 130 DEG C, rises to 200 ~ 210 DEG C with the heating rate of 5 ~ 20 DEG C/min, then rises to 220 ~ 230 DEG C with the heating rate of 3 ~ 6 DEG C/min, keeps 3 ~ 5 minutes.
Described polarity capillary chromatographic column can adopt HP-20M, DB-WAX or PEG-20M etc.
Internal standard substance solution described in the present invention recommends the acetone soln adopting fatty acid ester, and in requiring, mark peak is positioned between component peaks to be measured, without covering.Select the acetone soln of Ester to make interior mark ratio acid more stable, the long period can be preserved under refrigerated conditions and never degenerate.The acetone soln concentration of described fatty acid ester is between 2 ~ 3g/L.Described fatty acid ester can be carbon number be 16 ~ 24 fatty acid methyl ester or other ester class, such as: methyl margarate, arachic acid methyl esters etc.
In step of the present invention (4), the correction factor of each antiseptic to be measured is the series standard solution by the preservative component various to be measured by the internal standard substance solution containing 0.1 ~ 2.0g/L, records under the GC conditions of identical setting.
Ether of the present invention has to pass through liquor kalii iodide inspection, must not contain superoxide, otherwise easily cause sorbic acid measurement result on the low side.
The invention has the advantages that:
(1) accuracy of detection is high: the present invention adopts internal standard method, effectively reduce the error that the various factors such as concentration because of sample size, solvent loss, testing sample causes, also can not have an impact to result even if condition determination slightly changes, according to quantified by external standard method, then very high to the requirement of instrument apparatus and human users.
(2) running time is short: the present invention can simultaneously for the detection of Determination of Preservatives, only carry out as extractant the mixed liquor that disposable extraction obtains Determination of Preservatives with ether, pre-service and mensuration need not be carried out respectively by relevant GB, the sample pretreatment time shortens greatly than standard method, therefore can substantially reduce detection time.
(3) low being easy to of cost is promoted: the present invention is easy and simple to handle, less demanding to operating personnel, take hand sampling, utility configures general detecting instrument and apparatus, just can obtain ideal measurement result, higher-priced detecting instrument is configured without the need to height, as a rule, a set of gas chromatograph price is tens thousand of unit, and some instrument only automatic sampler one just tens thousand of unit of need, therefore, the present invention has saved the investment of instrument aspect greatly.In addition, pre-service need not be carried out respectively, save the consumption of reagent, further save testing cost.
(4) condition that polar stationary phase constant temperature of the present invention is separated can also be used for, to the fatty acid composition conventional analysis of edible vegetable oil, can realizing alternately measuring two test items, improve the utilization factor of instrument on same instrument.
accompanying drawing illustrates:
Fig. 1 is the capillary gas chromatography chromatogram of the embodiment of the present invention one;
Fig. 2 is the capillary gas chromatography chromatogram of the embodiment of the present invention two;
Fig. 3 is the capillary gas chromatography chromatogram of the embodiment of the present invention three;
Fig. 4 is the capillary gas chromatography chromatogram of the embodiment of the present invention four.
Embodiment
In order to understand essence of an invention better, describe the technology contents of invention below in detail by embodiment, but content of the present invention is not limited thereto.
embodiment one
1. chromatographic condition:
The gas chromatograph of configuration fid detector;
Capillary chromatographic column is HP-20M (25 mm × 0.30 μm, m × 0.32)
Column temperature 200 DEG C, vaporizer and sensing chamber are 220 DEG C
Hand sampling 1.0 μ l
Carrier gas is high pure nitrogen, column cap pressure 0.07Mpa, split ratio 100:1
2. correction factor measures
Preparing standard solution: accurately take benzoic acid, each 0.2g of sorbic acid, is settled to 100ml with acetone solution;
Preparation inner mark solution: accurately take methyl margarate 0.2g, is settled to 100ml with acetone solution;
Preparation standard uses solution: get appropriate standard solution and mix with inner mark solution, interior mark concentration is 0.4g/L, standard substance concentration is then respectively 0.2,0.4,0.6,0.8,1.0g/L.
Under above-mentioned chromatographic condition, with series standard solution sample introduction, with peak area ratio and concentration ratio drawing standard curve, obtain the correction factor of benzoic acid and sorbic acid, set up corresponding interior mark analytical approach.
3. sample preparation
1. dark soy sauce sample 1.0g is taken, be accurate to 0.001g, add the sodium chloride solution of 1.5g 200g/L again, be placed in 25ml tool plug test tube, accurately add 0.5ml inner mark solution, then add 0.5ml hydrochloric acid solution (1+1), mixing, divide 2 extractions with 30ml ether, each jolting 1 ~ 2min, the upper solution of twice extraction gained is incorporated in another 50ml tool plug test tube.
2. in the upper solution of gained, add the sodium bisulfate of 4ml 20g/L, fully vibrate 1 ~ 2min, leaves standstill 10 ~ 15min, then absorbs lower floor's solution with sharp mouth suction pipe, then repeat this step once to the upper solution retained.
3. step 2. in gained upper solution in add 5g anhydrous sodium sulfate, fully vibrate 1 ~ 2min, by solution impouring round-bottomed flask, be placed in nitrogen flushing in 40 ~ 45 DEG C of water-baths and be concentrated into about 0.5ml, add 2.0ml acetone along wall, move in 2ml sample bottle, machine of keeping supplying is used.
4. sample determination
Using under the chromatographic condition that solution is identical with standard, choose corresponding interior mark analytical approach, sample introduction measures, and read measurement result from chromatographic work station, chromatogram as shown in Figure 1.
embodiment two
1. chromatographic condition:
The gas chromatograph of configuration fid detector;
Capillary chromatographic column is PEG-20M (30 mm × 0.25 μm, m × 0.32)
Column temperature 210 DEG C, vaporizer is 230 DEG C with detecting room temperature
Hand sampling 0.5 μ l
Carrier gas is high pure nitrogen, column cap pressure 0.07Mpa, split ratio 50 ﹕ 1
2. correction factor measures
Preparing standard solution: accurately take benzoic acid, sorbic acid, methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, each 0.2g of propylparaben, is settled to 100ml with acetone solution;
Preparation inner mark solution: accurately take arachic acid methyl esters 0.2g, is settled to 100ml with acetone solution;
Preparation standard uses solution: get appropriate standard solution and mix with inner mark solution, interior mark concentration is 0.4g/L, the concentration of benzoic acid and sorbic acid is then respectively 0.2,0.4,0.6,0.8,1.0g/L, the concentration of methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, propylparaben is then respectively 0.05,0.1,0.15,0.2,0.25g/L.
Under above-mentioned chromatographic condition, solution sample introduction is used with series standard, with peak area ratio and concentration ratio drawing standard curve, obtain the correction factor of benzoic acid, sorbic acid, methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, propylparaben, set up corresponding interior mark analytical approach.
3. sample preparation
1. light soy sauce sample 2.5g is taken, be accurate to 0.001g, be placed in 25ml tool plug test tube, accurately add 0.5ml inner mark solution, add 0.5ml hydrochloric acid solution (1+1) again, mixing, divides 2 extractions with 25ml ether, each jolting 1 ~ 2min, is incorporated to the upper solution of twice extraction gained in another 50ml tool plug test tube.
2. in the upper solution of gained, add the sodium bisulfate of 5ml 20g/L, fully vibrate 1 ~ 2min, leaves standstill 10 ~ 15min, then absorbs lower floor's solution with sharp mouth suction pipe, then repeat this step once to the upper solution retained.
3. step 2. in gained upper solution in add 5g anhydrous sodium sulfate, fully vibrate 1 ~ 2min, by solution impouring round-bottomed flask, be placed in nitrogen flushing in 40 ~ 45 DEG C of water-baths and be concentrated into about 0.5ml, add 2.0ml acetone along wall, move in 2ml sample bottle, machine of keeping supplying is used.
4. sample determination
Using under the chromatographic condition that solution is identical with standard, choose corresponding interior mark analytical approach, sample introduction measures, and read measurement result from chromatographic work station, chromatogram as shown in Figure 2.
embodiment three
1. chromatographic condition:
The gas chromatograph of configuration fid detector;
Capillary chromatographic column is PEG-20M (30 mm × 0.25 μm, m × 0.32)
Column temperature 200 DEG C, vaporizer is 230 DEG C with detecting room temperature
Hand sampling 0.6 μ l
Carrier gas is high pure nitrogen, column cap pressure 0.06Mpa, split ratio 100 ﹕ 1
2. correction factor measures
Preparing standard solution: accurately take benzoic acid, sorbic acid, each 0.2g of dehydroactic acid, is settled to 100ml with acetone solution;
Preparation inner mark solution: accurately take methyl margarate 0.2g, is settled to 100ml with acetone solution;
Preparation standard uses solution: get appropriate standard solution and mix with inner mark solution, interior mark concentration is 0.4g/L, the concentration of benzoic acid and sorbic acid is then respectively 0.2,0.4,0.6,0.8,1.0g/L, the concentration of dehydroactic acid is then 0.05,0.1,0.15,0.2,0.25g/L.
Under above-mentioned chromatographic condition, use solution sample introduction with series standard, with peak area ratio and concentration ratio drawing standard curve, obtain the correction factor of benzoic acid, sorbic acid, dehydroactic acid, set up corresponding interior mark analytical approach.
3. sample preparation
1. light soy sauce sample 2.0g is taken, be accurate to 0.001g, be placed in 25ml tool plug test tube, accurately add 0.5ml inner mark solution, add 0.3ml hydrochloric acid solution (1+1) again, mixing, divides 2 extractions with 20ml ether, each jolting 1 ~ 2min, is incorporated to the upper solution of twice extraction gained in another 50ml tool plug test tube.
2. in the upper solution of gained, add the sodium bisulfate of 3ml 20g/L, fully vibrate 1 ~ 2min, leaves standstill 10 ~ 15min, absorbs lower floor with sharp mouth suction pipe, then repeat this step once to the upper solution retained.
3. step 2. in gained upper solution in add 5g anhydrous sodium sulfate, fully vibrate 1 ~ 2min, by solution impouring round-bottomed flask, be placed in nitrogen flushing in 40 ~ 45 DEG C of water-baths and be concentrated into about 0.5ml, add 2.0ml acetone along wall, move in 2ml sample bottle, machine of keeping supplying is used.
4. sample determination
Using under the chromatographic condition that solution is identical with standard, choose corresponding interior mark analytical approach, extracting sample solution sample introduction measures, and read measurement result from chromatographic work station, chromatogram as shown in Figure 3.
embodiment four
1. chromatographic condition:
The gas chromatograph of configuration fid detector;
Capillary chromatographic column is DB-WAX (30 mm × 0.25 μm, m × 0.32)
Vaporizer is 240 DEG C with detecting room temperature
Initial temperature 130 DEG C, rises to 210 DEG C with the heating rate of 15 DEG C/min, then rises to 230 DEG C with the heating rate of 5 DEG C/min, keeps 3 minutes.
Hand sampling 0.4 μ l
Carrier gas is high pure nitrogen, column cap pressure 0.08Mpa, split ratio 50 ﹕ 1
2. correction factor measures
Preparing standard solution: accurately take benzoic acid, sorbic acid, methyl p-hydroxybenzoate, each 0.2g of ethyl-para-hydroxybenzoate, is settled to 100ml with acetone solution;
Preparation inner mark solution: accurately take methyl margarate 0.2g, is settled to 100ml with acetone solution;
Preparation standard uses solution: get appropriate standard solution and mix with inner mark solution, interior mark concentration is 0.4g/L, the concentration of benzoic acid and sorbic acid is then respectively 0.2,0.4,0.6,0.8,1.0g/L, the concentration of methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate is then respectively 0.05,0.1,0.15,0.2,0.25g/L.
Under above-mentioned chromatographic condition, solution sample introduction is used with series standard, with peak area ratio and concentration ratio drawing standard curve, obtain the correction factor of benzoic acid, sorbic acid, methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, set up corresponding interior mark analytical approach.
3. sample preparation
1. light soy sauce sample 2.5g is taken, be accurate to 0.001g, be placed in 25ml tool plug test tube, accurately add 0.5ml inner mark solution, add 0.6ml hydrochloric acid solution (1+1) again, mixing, divides 2 extractions with 40ml ether, each jolting 1 ~ 2min, is incorporated to the upper solution of twice extraction gained in another 50ml tool plug test tube.
2. in the upper solution of gained, add 5ml 20g/L sodium bisulfate, fully vibrate 1min, leaves standstill 10 ~ 15min, then absorbs lower floor's solution with sharp mouth suction pipe, then repeat this step once to the upper solution retained.
3. step 2. in gained upper solution in add 5g anhydrous sodium sulfate, fully vibrate 1 ~ 2min, by solution impouring round-bottomed flask, be placed in nitrogen flushing in 40 ~ 45 DEG C of water-baths and be concentrated into about 0.5ml, add 2.5ml acetone along wall, dissolved residue, pipetting 2ml solution enters in sample bottle, and machine of keeping supplying is used.
4. sample determination
Using under the chromatographic condition that solution is identical with standard, choose corresponding interior mark analytical approach, extracting sample solution sample introduction measures, and read measurement result from chromatographic work station, chromatogram as shown in Figure 4.
Be described in detail method provided by the present invention above, apply specific case herein and set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping; Meanwhile, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (4)
1. the method for various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce, it is characterized in that, it comprises the following steps:
(1) soy sample is taken;
(2) internal standard substance solution is added in the sample to which, then acidifying is carried out successively, extracted by ether, purification dewaters and concentration, obtain sample solution: soy sample is placed in tool plug container, accurately add 0.3 ~ 0.7ml inner mark solution, add 0.3 ~ 0.7ml hydrochloric acid solution again, mixing, 2 extractions are divided with 20 ~ 40ml ether, merge twice upper solution, then in the upper solution of gained, 3 ~ 5ml sodium bisulfate is added, vibration, carry out washing, purifying, leave standstill, in upper solution, add 3 ~ 7g anhydrous sodium sulfate after removing lower floor's solution dewater, then in 40 ~ 45 DEG C of water-baths, nitrogen flushing is concentrated into 0.1 ~ 1ml, use 2 ~ 2.5ml acetone diluted again, sample solution, described internal standard substance solution adopts the acetone soln of the fatty acid ester of concentration between 2 ~ 3g/L, described fatty acid ester to be carbon number be 16 ~ 24 fatty acid methyl ester,
(3) sample solution got in step (2) carries out gas chromatographic analysis, obtains chromatogram analysis data, GC conditions: polarity capillary chromatographic column HP-20M, DB-WAX or PEG-20M, constant temperature 200 ~ 220 DEG C or temperature programme; Constant current or constant voltage, sample introduction 0.5 ~ 1.0 μ l manually or automatically, carrier gas is high pure nitrogen, column cap pressure 0.05 ~ 1Mpa, split ratio 50 ~ 100 ﹕ 1, temperature programme condition is wherein: initial temperature 120 ~ 130 DEG C, rises to 200 ~ 210 DEG C with the heating rate of 5 ~ 20 DEG C/min, rise to 220 ~ 230 DEG C with the heating rate of 3 ~ 6 DEG C/min again, keep 3 ~ 5 minutes;
(4) by the chromatogram analysis data of the acquisition of step (3) and the comparison of predetermined antiseptic normal data, the content of various antiseptic in soy sauce is obtained.
2. the method for various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce according to claim 1, is characterized in that, take the consumption of described soy sample in described step (1) according to different soy sauce classification.
3. the method for various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce according to claim 2, is characterized in that, when the soy sauce in described step (1) is dark soy sauce class soy sauce, need carry out pre-service to dark soy sauce class soy sauce.
4. the method for various antiseptic content in capillary gas chromatography internal standard method Simultaneously test soy sauce according to claim 3, it is characterized in that, described pre-service is: in dark soy sauce class soy sample, add sodium chloride solution dilution 1 ~ 2.5 times.
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| CN102662009B (en) * | 2012-04-25 | 2014-02-26 | 辽宁省食品药品检验所 | Method for quickly determining content of additive of plurality of types in food |
| CN102998389B (en) * | 2012-11-23 | 2014-07-09 | 浙江赞宇科技股份有限公司 | Gas chromatography detection method of corrosion removers in food |
| CN103076407B (en) * | 2012-12-26 | 2014-07-09 | 通标标准技术服务有限公司 | Fast detection method for food preservative agent and antioxidant |
| CN103134870B (en) * | 2013-02-01 | 2014-09-03 | 浙江工业大学 | Method for measuring sorbic acid and benzoic acid in foodstuff |
| CN103743831A (en) * | 2013-12-21 | 2014-04-23 | 广西科技大学 | Method for detecting sorbic acid serving as food preservative |
| CN103760249A (en) * | 2013-12-23 | 2014-04-30 | 广西科技大学 | Detection method of deoxidation acetic acids of food antiseptics |
| CN106404936A (en) * | 2016-08-25 | 2017-02-15 | 宁波检验检疫科学技术研究院 | Method used for detecting pentyl p-hydroxybenzoate in washing products |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101526509A (en) * | 2009-05-04 | 2009-09-09 | 佛山市海天调味食品有限公司 | Method for rapidly determining content of preservatives in condiment |
| KR100942314B1 (en) * | 2009-03-18 | 2010-02-17 | 대한민국 | Measurement method for purity of didecyl-dimethyl-ammonium chloride using hplc-ms |
-
2011
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-
2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100942314B1 (en) * | 2009-03-18 | 2010-02-17 | 대한민국 | Measurement method for purity of didecyl-dimethyl-ammonium chloride using hplc-ms |
| CN101526509A (en) * | 2009-05-04 | 2009-09-09 | 佛山市海天调味食品有限公司 | Method for rapidly determining content of preservatives in condiment |
Non-Patent Citations (2)
| Title |
|---|
| 毛细管气相色谱内标法同时测定食品中8种防腐剂;鲍忠定 等;《分析化学》;20040229;第32卷(第2期);270页全文 * |
| 气相色谱内标法测定食品中的防腐剂苯甲酸和山梨酸;黎清金 等;《农产品加工·学刊》;20090630(第6期);103页1.3.1-1.3.2节 * |
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