CN103616448A - Method and system for detecting food additive - Google Patents
Method and system for detecting food additive Download PDFInfo
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- CN103616448A CN103616448A CN201310627315.4A CN201310627315A CN103616448A CN 103616448 A CN103616448 A CN 103616448A CN 201310627315 A CN201310627315 A CN 201310627315A CN 103616448 A CN103616448 A CN 103616448A
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Abstract
The invention relates to an analysis method for rapidly determining benzoic acid, sorbic acid and saccharin sodium in food by utilizing a HPLC (high performance liquid chromatography). The method adopts a C18 reverse high-efficiency liquid-phase chromatographic column, utilizes a methanol and ammonium acetate solution as a mobile phase for eluting and utilizes an ultraviolet detector to detect at the wavelength of 230nm. When the ratio of the methanol to ammonium acetate (V/V) in the mobile phase is 40: 60, various components can be well separated, the chromatographic peak resolution can reach more than 3.0, the chromatographic peak shape is sharp, and the retention time is relatively short. The RSD (Relative Standard Deviation) of the chromatographic peak area and the retention time is less than 1 percent. The method is good in accuracy and precision. Under the chromatographic condition, real samples of beverage, seasoning and the like are detected, the detection results show that the HPLC method under the chromatographic condition is rapid, accurate and good in repetition, and the HPLC method can be used as a reference method for qualitative and quantitative analysis of preservatives and sweetening agents in the food.
Description
Technical field
The invention belongs to food analysis field, relate to particularly a kind of detection method of food additives.
background technologyfood additives refer to as improving food color and joining chemosynthesis material or the natural materials in food for anticorrosion with needs processing technology.At present, along with kind and the constantly increase of use of food additives, its security is subject to extensive concern.The food that often edible additive exceeds standard, can cause stimulation to human body alimentary canal, and severe patient also can liver injury, causes food poisoning, so will strictly control its use amount.Benzoic acid, sorbic acid and saccharin sodium are conventional food additives, state health standards strict regulations their use limit the quantity of.At present, in food, the conventional assay method of benzoic acid, sorbic acid and saccharin sodium has vapor-phase chromatography (GC), thin-layered chromatography (TLC) and high performance liquid chromatography (HPLC); The mensuration of saccharin sodium has GC method, TLC method and ion selective electrode method (ISE).TLC method complicated operation, only can semi-quantitative analysis; ISE method needs specific installation; HPLC method is widely used, and can to 3 kinds of adjuvants, measure simultaneously.GB GB/T23495-2009 is exactly the content that adopts benzoic acid, sorbic acid and saccharin sodium in food by HPLC.But national standard method is longer detection time in real work.
Summary of the invention
The rapid assay methods that the object of this invention is to provide multiple additives content in a kind of food.By the optimization to the chromatographic condition of HPLC, set up a kind of HPLC method of sorbic acid, benzoic acid and saccharin sodium in fast detecting food, and for the detection of actual sample.Adopt method of the present invention, fast, accurately, improved detection efficiency, reduced testing cost.To achieve these goals, the technical solution used in the present invention is: the detection method of multiple additives in a kind of food, specifically comprises:
1) the preparation saccharin sodium standard inventory solution of contrast liquid, accurately takes 1.0000g through 120 ℃ of saccharin sodiums of drying after 4h, is dissolved in water, and is settled to 100.0mL.Benzoic acid or sorbic acid standard inventory solution, accurately take 0.5000g benzoic acid or sorbic acid, adds sodium bicarbonate solution 50mL, and heating for dissolving, is settled to 100mL.Standard is mixed use solution, draws and accurately draws each standard reserving solution 5.0mL in 100mL volumetric flask, is settled to scale, filters ultrasonic degas.
2) processing of sample
Carbonated and tea beverage directly weigh, and tepor stirs and removes carbon dioxide, with ammoniacal liquor (volume ratio is 1: 1) adjust pH approximately 7, adds water constant volume 25ml, through membrane filtration, and ultrasonic degas.Fruit juice class sample is by the abundant centrifugation of whole samples, gets supernatant, then weighs, and with ammoniacal liquor (volume ratio is 1: 1) adjust pH approximately 7, adds water constant volume 25ml, through membrane filtration, and ultrasonic degas.Condiment class sample is direct weighing, adds water constant volume 10ml, through membrane filtration, and ultrasonic degas.3) selection of condition determination:
ODS C18 chromatographic column (250mm * 4.6mm, 5 μ m), ultraviolet detects wavelength 230nm, sample size 10 μ L.Mobile phase: V (methyl alcohol): V (ammonium acetate solution) (0.02mol/L)=40: 60, flow velocity 1.0mL/min, 35 ℃ of column temperatures.4) operation steps:
HPLC methyl alcohol and 0.02mol/L ammonium acetate are filtered mobile phase through solvent filtration apparatus respectively to ultrasonic degas.Each 10 μ L of sample thief treating fluid, by above-mentioned chromatographic condition, inject respectively high performance liquid chromatograph analysis.
The invention has the beneficial effects as follows: by method of the present invention, realized the fast detecting to several foods adjuvant sorbic acid, benzoic acid and saccharin sodium.The 20min in GB shortened in 5min and completed the detection time that makes several adjuvants, and each component all obtains good separation, the HPLC method that the testing result of actual sample is shown to this chromatographic condition is quick, accurate, favorable reproducibility, the application that can obtain in varieties of food items detects.
Embodiment
1, optimize chromatography condition is according to national standard, when methyl alcohol and ammonium acetate ratio are 5: 95, benzoic retention time is 10.315min, the retention time of sorbic acid is 14.282min, the retention time of saccharin sodium is 18.382min, in order to shorten detection time, improve detection efficiency, select to adjust the ratio of 2 kinds of solvents.When the ratio (V/V) of mobile phase methanol and ammonium acetate changed to 55: 45 from 5: 95, find the appearance time of the direct impact analysis thing of volume of methyl alcohol in mobile phase, methyl alcohol volume increases, and the retention time of all analytes all shortens, wherein particularly evident with saccharin sodium.When the ratio (V/V) of mobile phase methanol and ammonium acetate of adjusting is 40: 60, in 5min, can complete detection, each component all obtains good separation, and chromatographic peak degree of separation reaches more than 3.0, and tailing factor is little, and chromatographic peak type is sharp-pointed.Peak sequence is saccharin sodium, benzoic acid, sorbic acid, goes out peak retention time and is respectively 3.587,4.176 and 4.788min.2, the uv-absorption maximum wavelength of the selection asccharin of detection wavelength is that 202nm, benzoic acid are that 230nm, sorbic acid are 253nm.The maximum absorption wavelength of asccharin and the cutoff wavelength of methyl alcohol are close, if adopt 202nm as detecting wavelength, the absorbance of mobile phase own is too large.If with 253nm as detecting wavelength, a little less than the absorption too of asccharin.The comprehensive above 230nm of employing is as detecting wavelength.3, typical curve pipette respectively saccharin sodium and benzoic acid, sorbic acid standard reserving solution each 0.00,0.25,0.50,1.00,2.00,4.00mL is in 10mL volumetric flask, with distilled water, be settled to scale, obtain benzoic acid, sorbic acid concn is 0,0.00625,0.0125,0.025,0.05,0.1g/L and saccharin sodium concentration are 0,0.0125,0.025,0.05,0.1,0.2g/L standard series.By the chromatographic condition of optimizing, measure peak area, the working curve of 3 kinds of adjuvants and correlativity are in Table 1.
The working curve of 3 kinds of adjuvants of table 1
| Adjuvant | Related coefficient | Working curve inspection | Detection limit |
| Benzoic acid | 0.9999 | Y=(3.179X+0.002)×10 7 | 5.36 |
| Sorbic acid | 0.9999 | Y=(6.220X+0.004)×10 7 | 0.612 |
| Saccharin sodium | 0.9999 | Y=(2.306X+0.007)×10 7 | 0.321 |
From table 1, the linear relationship of benzoic acid, sorbic acid, saccharin sodium calibration curve good (related coefficient is all greater than 0.99900).4, precision, accuracy test are being optimized under chromatographic condition, (concentration is respectively 0.025 to draw continuously the mixed liquid of benzoic acid, sorbic acid and saccharin sodium standard, 0.025,0.05g/L) 10 μ L injecting chromatographs, measure respectively each component retention time, peak height and peak area, calculate the relative standard deviation (RSD) of standard model.The RSD scope of benzoic acid, sorbic acid and saccharin sodium retention time is 0.092% ~ 0.122%; The RSD scope of peak area is 0.889% ~ 0.979%.Chinese Pharmacopoeia HPLC regulation, impurity content is lower than 0.5% sample, and the RSD of chromatographic peak area should be less than 10%; Impurity content is at 0.5% ~ 2% sample, and the RSD of chromatographic peak area should be less than 5%; The sample that impurity content is greater than 2%, the RSD of peak area should be less than 2%.Therefore, show that the method has good accuracy and precision.
5, concrete case study on implementation
Embodiment 1
Carbonated and tea beverage directly take beverage 5.000g, put into small beaker, and tepor stirs and removes carbon dioxide, with ammoniacal liquor (volume ratio is 1: 1) adjust pH approximately 7.Add water and be settled to 25mL, through membrane filtration, ultrasonic degas.HPLC methyl alcohol and 0.02mol/L ammonium acetate are filtered mobile phase through solvent filtration apparatus respectively to ultrasonic degas.Each 10 μ L of sample thief treating fluid, ODS C18 chromatographic column (250mm * 4.6mm, 5 μ m), ultraviolet detects wavelength 230nm, sample size 10 μ L.Mobile phase: V (methyl alcohol): V (ammonium acetate solution) (0.02mol/L)=40: 60, flow velocity 1.0mL/min, 35 ℃ of column temperatures.In certain brand soda, benzoic acid detected, content is 0.01.g/L; In tea beverage, do not detect 3 kinds of adjuvants.Embodiment 2
The abundant centrifugation of the whole samples of fruit juice class class sample, gets supernatant.Take respectively fruit juice 5.000g, use respectively ammoniacal liquor (volume ratio is 1: 1) adjust pH approximately 7, add water and be settled to 25mL, through membrane filtration, ultrasonic degas.HPLC methyl alcohol and 0.02mol/L ammonium acetate are filtered mobile phase through solvent filtration apparatus respectively to ultrasonic degas.Each 10 μ L of sample thief treating fluid, ODS C18 chromatographic column (250mm * 4.6mm, 5 μ m), ultraviolet detects wavelength 230nm, sample size 10 μ L.Mobile phase: V (methyl alcohol): V (ammonium acetate solution) (0.02mol/L)=40: 60, flow velocity 1.0mL/min, 35 ℃ of column temperatures.In certain brand fruit juice, sorbic acid detected, content is 0.002g/L.
Embodiment 3
Condiment class sample takes soy sauce 10.0290g, and directly add water and be settled to 10mL, through membrane filtration, ultrasonic degas.HPLC methyl alcohol and 0.02mol/L ammonium acetate are filtered mobile phase through solvent filtration apparatus respectively to ultrasonic degas.Each 10 μ L of sample thief treating fluid, ODS C18 chromatographic column (250mm * 4.6mm, 5 μ m), ultraviolet detects wavelength 230nm, sample size 10 μ L.Mobile phase: V (methyl alcohol): V (ammonium acetate solution) (0.02mol/L)=40: 60, flow velocity 1.0mL/min, 35 ℃ of column temperatures.In certain brand soy sauce, benzoic acid detected, content is 0.02g/L.
We utilize HPLC method, separated with C18 reverse chromatograms post, UV-detector detects, by changing methyl alcohol and ammonium acetate (V/V) ratio optimization testing conditions in mobile phase, when V (methyl alcohol)/V (ammonium acetate) is when being 31: 69, realized the fast detecting to 3 kinds of food additives sorbic acids, benzoic acid and saccharin sodiums.The 20min in GB shortened in 5min and completed the detection time that makes 3 kinds of adjuvants.Under this chromatographic condition, each component all obtains good separation.The HPLC method that the testing result of actual sample is shown to this chromatographic condition is quick, accurate, favorable reproducibility, the application that can obtain in varieties of food items detects.
Claims (5)
1. a method that detects food additives, is characterized in that, comprises following methods:
The preparation of A, contrast liquid
The processing of B, sample
The selection of C, condition determination
D, operation steps.
2. a method for multiple additives content in food, is characterized in that, the concrete steps of the preparation of described steps A contrast liquid are as follows:
Saccharin sodium contrast liquid, accurately takes 1.0000g through 120 ℃ of saccharin sodiums of drying after 4h, is dissolved in water, and is settled to 100.0mL.Benzoic acid and sorbic acid contrast liquid, accurately take 0.5000g benzoic acid or sorbic acid, adds sodium bicarbonate solution 50mL, and heating for dissolving, is settled to 100mL.Standard is mixed contrast liquid, draws and accurately draws each standard control liquid 5.0mL in 100mL volumetric flask, is settled to scale, filters ultrasonic degas.
3. a method for multiple additives content in food, is characterized in that, the concrete steps of the processing of described step B sample are as follows:
Carbonated and tea beverage directly weigh 5ml, and tepor stirs and removes carbon dioxide, and with ammoniacal liquor (volume ratio is 1: 1) adjust pH approximately 7, add water and be settled to 25ml, through membrane filtration, ultrasonic degas.Fruit juice class sample is by the abundant centrifugation of whole samples, gets supernatant, then weighs 5ml, with ammoniacal liquor (volume ratio is 1: 1) adjust pH approximately 7, add water and be settled to 25ml, and through membrane filtration, ultrasonic degas.Condiment class sample is directly to weigh 5g, adds water and is settled to 10ml, and through membrane filtration, ultrasonic degas.
4. a method for multiple additives content in food, is characterized in that, the selection of described step C condition determination is specific as follows:
ODS C18 chromatographic column (250mm * 4.6mm, 5 μ m), ultraviolet detects wavelength 230nm, sample size 10 μ L.Mobile phase: V (methyl alcohol): V (ammonium acetate solution) (0.02mol/L)=40: 60, flow velocity 1.0mL/min, 35 ℃ of column temperatures.
5. a method for multiple additives content in food, is characterized in that, described step D operation steps is as follows:
HPLC methyl alcohol and 0.02mol/L ammonium acetate are filtered mobile phase through solvent filtration apparatus respectively to ultrasonic degas.Each 10 μ L of sample thief treating fluid, by above-mentioned chromatographic condition, inject respectively high performance liquid chromatograph analysis.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105044266A (en) * | 2015-08-10 | 2015-11-11 | 云南省食品药品检验所 | Method of detecting content of preservative in cosmetic |
| CN106353438A (en) * | 2016-11-30 | 2017-01-25 | 无锡艾科瑞思产品设计与研究有限公司 | Method for detecting sorbic acid in foods |
| CN106596803A (en) * | 2016-11-16 | 2017-04-26 | 方贵雄 | Method for detecting sorbic acid in food |
| CN107202724A (en) * | 2017-07-11 | 2017-09-26 | 安徽宏远职业卫生技术服务有限公司 | The sample pretreating method of preservative in a kind of detection fruit juice |
| CN107589188A (en) * | 2017-09-04 | 2018-01-16 | 浙江树人学院 | The separation of Vavle switching technology coupled HPLC while the method for detecting the carbohydrate in beverage, sweetener and preservative |
| CN108318600A (en) * | 2018-04-04 | 2018-07-24 | 深圳市宇驰检测技术股份有限公司 | A kind of detection method of food additives content |
| CN114137140A (en) * | 2017-01-13 | 2022-03-04 | 广西民族大学 | Method for synchronously detecting food additives and heavy metal content in food by reverse phase HPLC-ICP-MS method |
| CN115452963A (en) * | 2021-10-14 | 2022-12-09 | 王丽蓉 | Method for detecting mixed food additive in pickled vegetables |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105044266A (en) * | 2015-08-10 | 2015-11-11 | 云南省食品药品检验所 | Method of detecting content of preservative in cosmetic |
| CN106596803A (en) * | 2016-11-16 | 2017-04-26 | 方贵雄 | Method for detecting sorbic acid in food |
| CN106353438A (en) * | 2016-11-30 | 2017-01-25 | 无锡艾科瑞思产品设计与研究有限公司 | Method for detecting sorbic acid in foods |
| CN114137140A (en) * | 2017-01-13 | 2022-03-04 | 广西民族大学 | Method for synchronously detecting food additives and heavy metal content in food by reverse phase HPLC-ICP-MS method |
| CN107202724A (en) * | 2017-07-11 | 2017-09-26 | 安徽宏远职业卫生技术服务有限公司 | The sample pretreating method of preservative in a kind of detection fruit juice |
| CN107589188A (en) * | 2017-09-04 | 2018-01-16 | 浙江树人学院 | The separation of Vavle switching technology coupled HPLC while the method for detecting the carbohydrate in beverage, sweetener and preservative |
| CN107589188B (en) * | 2017-09-04 | 2020-03-17 | 浙江树人学院 | Method for simultaneously detecting saccharides, sweetening agents and preservatives in beverage by combining valve switching technology and chromatographic separation |
| CN108318600A (en) * | 2018-04-04 | 2018-07-24 | 深圳市宇驰检测技术股份有限公司 | A kind of detection method of food additives content |
| CN115452963A (en) * | 2021-10-14 | 2022-12-09 | 王丽蓉 | Method for detecting mixed food additive in pickled vegetables |
| CN115452963B (en) * | 2021-10-14 | 2023-07-25 | 王丽蓉 | Method for detecting mixed food additive in pickled vegetables |
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Application publication date: 20140305 |