CN103472170A - Method for detecting benzopyrene in edible oil - Google Patents
Method for detecting benzopyrene in edible oil Download PDFInfo
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- CN103472170A CN103472170A CN2013104106937A CN201310410693A CN103472170A CN 103472170 A CN103472170 A CN 103472170A CN 2013104106937 A CN2013104106937 A CN 2013104106937A CN 201310410693 A CN201310410693 A CN 201310410693A CN 103472170 A CN103472170 A CN 103472170A
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Abstract
The invention discloses a method for detecting benzopyrene in edible oil. The method comprises the following steps of weighing an oil sample; adding a potassium hydroxide ethanol water solution; vibrating a mixture until the mixture is clarified; saponifying the clarified mixture in a water bath at the temperature of 50 DEG C for 1 hour; cooling the mixture until the temperature decreases to room temperature, and adding water into a sample centrifugation tube; after the mixture and water are shaken uniformly, adding 15ml of normal hexane, performing uniform mixing and centrifugation, and washing two times by 5ml of ultrapure water; concentrating an extraction solution in a nitrogen blowing concentrator until the extraction solution is dried completely; making up to constant volume through a mixed solution consisting of 20 percent of tetrahydrofuran and 80 percent of acetonitrile; and performing filtration through a filtering membrane, and then determining a result through a high performance liquid chromatograph. The analysis method disclosed by the invention has the advantages of simplicity in operation, high stability and high recovery rate.
Description
Technical field
The invention belongs to the food analysis field, be specifically related to a kind of detection method of benzopyrene from edible oil.
Background technology
Benzopyrene claims again benzo (а) pyrene, and english abbreviation BaP is the organic compound that a class has obvious carcinogenesis.It is by a phenyl ring and a polycyclic arene compound that the pyrene molecule is combined into.After testing, nonexpondable high-temperature vegetable oil, the fried food overdoed all can produce B (a) P, Reusability high temperature frying mode, and the organic decomposes in food, form the carcinogenic compositions such as B (a) P through cyclisation, polymerization.
Benzene in food (а) pyrene is that polycyclic aromatic hydrocarbons contaminated trace analysis becomes an important topic, and the trace benzopyrene in Accurate Determining food is particularly important.The method of existing detection benzo (а) pyrene mainly contains: (1) fluorometry can be characterized by the characteristic fluorescence spectrum of benzo (а) pyrene, some complex mixture analyses are often occurred that spectrum is overlapped, are difficult for differentiating, even adopt some new technologies can improve resolution as synchronous fluorescence, fluorescence reciprocal, but the number that can differentiate is limited, often need sample is carried out to pre-separation and complex operation; (2) its separation method of liquid chromatography-detection technique of fluorescence is mostly gradient elution, although can realize the separation of palycyclic aromatic, but the method for liquid-liquid extraction need to expend a large amount of extra pure regents, and emulsion appears in extract sometimes, analysis time long (China's national standard is 60min), not only waste reagent but also easily cause error, and have the problem of baseline wander; (3) gas chromatography-mass spectrum (GC-MS) method can accurately be differentiated benzene (а) pyrene, but elution time long (30～60min); Also must regularly with titer, calibrate retention time, to the higher boiling PAHs gasification difficulty that contains 4～6 phenyl ring, can't carry out compartment analysis, also can't differentiate the different material with similar mass fragments spectrum; (4) enzyme-linked immune analytic method (ELISA) is to grow up in recent years to take the novel analytical technology that the specificity, reversibility association reaction of antigen and antibody be basis.But this method is measured PAH and is contrasted with the result that HPLC measures, and does not find false-negative sample, but exists 18% false positive sample to exist.
In having developed the method for multiple separation and detection PAH material at present, HPLC method and the application of GC-MS method are general, measuring accuracy is high, be suitable for standardization, but, for complicated food substrate, degree of separation is very restricted, often need to carry out complicated sample preparation, particularly in pre-treatment, to use activated alumina column to be separated, higher to the quality requirements of aluminium oxide.Wherein, GB GB/T22509-2008 " benzo (а) pyrene of oil in the mensuration of animal and plant fat benzopyrene " project detecting step is comparatively loaded down with trivial details, the activity of neutral alumina filler directly has influence on the stability of testing result, and it is unsuitable long standing time to regulate active neutral alumina, the convenience that impact detects.
Mensuration and the safety evaluation thereof of benzo (а) pyrene in the Guiyang fried food that high performance liquid chromatography and Yang Zhannan etc. deliver at " Food Science " magazine, adopting saponification method to remove grease is detected, effumability due to benzo (а) pyrene, if carry out saponification according to the method that adds hot reflux, very easily cause the volatilization of benzene benzo (а) pyrene and affect testing result, the present invention is optimized oily saponification temperature and saponification time, make testing process easy and simple to handle, save time, and guaranteed that testing result is accurate.
Summary of the invention
The technical problem to be solved in the present invention: for the complex pretreatment existed in prior art, stability is bad, and inspection range is narrow, add the problems such as the recovery is low, the present invention adopts saponification 1h in the water-bath of 50 ℃, has simple to operate, stablize, add the high advantage of the recovery.
The technical solution used in the present invention: the detection method of benzopyrene from edible oil comprises the following steps:
(1) method of pre-treatment: the oil sample that takes 0.5g, add the vibration of 5mL1mol/L potassium hydroxide ethanol water to clarification, continue vibration 1min, saponification 1h in the water-bath of 50 ℃, to be cooled to room temperature, add the 5ml ultrapure water in the sample centrifuge tube, shake up, add again the 15ml normal hexane, and mix on turbine mixer, centrifugal, supernatant is moved in test tube, and adding the normal hexane of 10ml in the sample centrifuge tube, the same step operation, by the extracted twice liquid merged, with 5ml ultrapure water washing 2 times, extract is placed in Nitrogen evaporator and is concentrated into dry, with tetrahydrofuran+acetonitrile=2+8 mixed solution 1.0mL constant volume, 0.45um after membrane filtration, upper machine is measured,
(2), with the high performance liquid chromatograph analysis of being furnished with fluorescence detector, obtain the test result of benzopyrene from edible oil.
Wherein, the chromatographic condition of high performance liquid chromatograph is mobile phase: acetonitrile: water=88:12; Flow velocity: 1.0ml/min; Column temperature: 30 ± 2 ℃; Chromatographic column model: EclipsePAH5 μ m4.6 * 250mm; Emission wavelength: 406nm(slit 10nm), excitation wavelength: 384nm (slit 10nm).
The present invention reaches beneficial effect: the prior art poplar comparatively approaching with the present invention accounts for " mensuration and the safety evaluation thereof of benzo in the fried food of Guiyang (а) pyrene " that deliver at " Food Science " magazine in south, adopting saponification method to remove grease is detected, effumability due to benzo (а) pyrene, carry out saponification if add the method for hot reflux according to document, very easily cause the volatilization of benzene benzo (а) pyrene and affect testing result, the present invention is optimized oily saponification temperature and saponification time, make testing process easy and simple to handle, save time, and guaranteed that testing result is accurate.Concrete beneficial effect illustrates by the data of following enforcement.
Embodiment
Embodiment 1
(1) repeated experiment
The detection method of benzopyrene from edible oil of the present invention comprises the following steps:
(1) method of pre-treatment: take respectively 0.3854g, 0.4699g, 0.5300 and 0.5521 tealeaves seed oil, add the vibration of 5mL1mol/L potassium hydroxide ethanol water to clarification, continue vibration 1min, saponification 1h in the water-bath of 50 ℃, to be cooled to room temperature, add the 5ml ultrapure water in the sample centrifuge tube, shake up, add again the 15ml normal hexane, and mix on turbine mixer, centrifugal, supernatant is moved in test tube, and adding the normal hexane of 10ml in the sample centrifuge tube, the same step operation, by the extracted twice liquid merged, with 5ml ultrapure water washing 2 times, extract is placed in Nitrogen evaporator and is concentrated into dry, be settled to 1ml with tetrahydrofuran+acetonitrile=2+8 mixed solution, after filtering membrane filtration, upper machine is measured,
(2) with the high performance liquid chromatograph analysis of being furnished with fluorescence detector, the chromatographic condition of high performance liquid chromatograph is mobile phase: acetonitrile: water=88:12; Flow velocity: 1.0ml/min; Column temperature: 30 ± 2 ℃; Chromatographic column model: EclipsePAH5 μ m4.6 * 250mm; Emission wavelength: 406nm(slit 10nm), excitation wavelength: 384nm (slit 10nm).
Result be can obtain according to the following result computing formula and 7.04ug/kg, 6.84ug/kg, 7.00ug/kg and 6.85ug/kg are respectively.
Embodiment 2
(2) add recovery test
According to the experimental technique of embodiment 1, after taking the sample identical with embodiment 1, add the mark liquid of BaP, concrete addition is in Table 1, and follow-up pre-treatment and instrumental analysis are identical with embodiment 1, and test result is as shown in table 1.
Calculate the recovery of standard addition theoretical formula with concentration value:
P=（c2－c1）/c3×100%
In formula: P is recovery of standard addition; C1 is sample solution concentration, i.e. Specimen Determination value, c1=m1/V1; C2 is the mark-on sample solution concentration, i.e. mark-on Specimen Determination value, c2=m2/V2; C3 is for adding scalar, c3=c0 * V0/V2:m=c0 * V0; M1 is the content of material in sample; M2 is the content of material in the mark-on sample; M is the content of material in the mark-on volume; V1 is volume of sample; V2 is the mark-on volume of sample, V2=V1+V0; V0 is for adding scalar product; C0 is the mark-on concentration of standard solution.
Table 1 interpolation recovery experiment of the present invention result
| Numbering | The heavy g of oil | Add scalar ng | Recovery % |
| 1 | 0.5214 | 1.032 | 106.2 |
| 2 | 0.4946 | 1.032 | 109.4 |
| 3 | 0.5809 | 2.58 | 91.7 |
| 4 | 0.4552 | 5.16 | 104.6 |
| 5 | 0.5588 | 10.32 | 103.3 |
| 6 | 0.5596 | 10.32 | 103.7 |
Embodiment 3
Experimental technique in " mensuration and the safety evaluation thereof of benzo in the fried food of Guiyang (а) pyrene " that the present invention and Yang Zhannan etc. deliver at " Food Science " magazine is the contrast experiment, the key distinction is that the present invention adopts saponification 1h in the water-bath of 50 ℃, and above-mentioned document adopts backflow saponification 1h in the water-bath of 80 ℃, done respectively the sample blank experiment and added recovery experiment, experimental result is as shown in table 2.The interpolation recovery of the present invention is between 96.4～103.7%, and the interpolation recovery that adopts above-mentioned literature method is between 65.2～77.0%, illustrate that saponification temperature and time in pre-treatment of the present invention obviously is better than documents, improved the accuracy of data, and shortened the time of experiment.
The contrast test of table 2 the present invention and documents
Claims (2)
1. the detection method of a benzopyrene from edible oil is characterized in that: comprise the following steps:
(1) method of pre-treatment: the oil sample that takes 0.5g, add the vibration of 5mL1mol/L potassium hydroxide ethanol water to clarification, continue vibration 1min, saponification 1h in the water-bath of 50 ℃, to be cooled to room temperature, add the 5ml ultrapure water in the sample centrifuge tube, shake up, add again the 15ml normal hexane, and mix on turbine mixer, centrifugal, supernatant is moved in test tube, and adding the normal hexane of 10ml in the sample centrifuge tube, the same step operation, by the extracted twice liquid merged, with 5ml ultrapure water washing 2 times, extract is placed in Nitrogen evaporator and is concentrated into dry, with tetrahydrofuran+acetonitrile=2+8 mixed solution constant volume, after filtering membrane filtration, upper machine is measured,
(2), with the high performance liquid chromatograph analysis of being furnished with fluorescence detector, obtain the test result of benzopyrene from edible oil.
2. the detection method of a kind of benzopyrene from edible oil as claimed in claim 1, it is characterized in that: the chromatographic condition of high performance liquid chromatograph is mobile phase: acetonitrile: water=88:12; Flow velocity: 1.0ml/min; Column temperature: 30 ± 2 ℃; Chromatographic column model: EclipsePAH, 5 μ m4.6 * 250mm; Emission wavelength: 406nm, excitation wavelength: 384nm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103712839A (en) * | 2014-01-03 | 2014-04-09 | 上海安谱科学仪器有限公司 | Sample processing method for measuring content of benzo(a)pyrene by virtue of small column |
| CN103869014A (en) * | 2014-03-19 | 2014-06-18 | 山东鲁花集团有限公司 | Extraction method for benzo(a)pyrene in edible oil |
| CN105203373A (en) * | 2015-09-10 | 2015-12-30 | 上海安谱实验科技股份有限公司 | Method for simply, fast, efficiently and stably testing benzopyrene in food |
| CN105223301A (en) * | 2015-09-23 | 2016-01-06 | 成都艾比科生物科技有限公司 | A kind of method for measuring benzopyrene content in vegetable oil |
| CN105866288A (en) * | 2016-05-10 | 2016-08-17 | 芜湖雨耕山食品检测有限公司 | Method of utilizing high performance liquid chromatography to detect benzo (a) pyrene in edible oil |
| CN105954369A (en) * | 2016-04-19 | 2016-09-21 | 中华人民共和国吉林出入境检验检疫局 | Analysis method for determining benzo(alpha)pyrene in water through ionic liquid homogeneous liquid-liquid extraction and high-performance liquid chromatography |
| CN106053371A (en) * | 2016-05-17 | 2016-10-26 | 中国科学院青岛生物能源与过程研究所 | Method for rapidly detecting benzopyrene in plant oil |
| CN108645689A (en) * | 2018-04-28 | 2018-10-12 | 山东省食品药品检验研究院 | A kind of device and method for BaP detection pre-treatment |
| CN110609096A (en) * | 2019-09-02 | 2019-12-24 | 宁波中盛产品检测有限公司 | Rapid extraction and purification method for 4 polycyclic aromatic hydrocarbon compounds in edible oil and detection application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100551700B1 (en) * | 2003-10-06 | 2006-02-13 | 경기도보건환경연구원 | Assay methods of organic matters |
| CN102288720A (en) * | 2011-07-26 | 2011-12-21 | 中国林业科学研究院亚热带林业研究所 | Method for detecting benzo(a)pyrene of oiltea camellia seed oil |
-
2013
- 2013-09-10 CN CN2013104106937A patent/CN103472170A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100551700B1 (en) * | 2003-10-06 | 2006-02-13 | 경기도보건환경연구원 | Assay methods of organic matters |
| CN102288720A (en) * | 2011-07-26 | 2011-12-21 | 中国林业科学研究院亚热带林业研究所 | Method for detecting benzo(a)pyrene of oiltea camellia seed oil |
Non-Patent Citations (3)
| Title |
|---|
| 吴雪美: "食品中多环芳烃类物质分析方法比较研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 李燕艳 等: "RP—HPLC法测定食用油中苯并(a)芘的含量", 《中国粮油学报》 * |
| 董广彬 等: "《中华人民共和国国家标准 GB／T 22509—2008》", 4 November 2008, 中华人民共和国国家质量监督检验检疫总局，中国国家标准化管理委员会 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103712839A (en) * | 2014-01-03 | 2014-04-09 | 上海安谱科学仪器有限公司 | Sample processing method for measuring content of benzo(a)pyrene by virtue of small column |
| CN103869014A (en) * | 2014-03-19 | 2014-06-18 | 山东鲁花集团有限公司 | Extraction method for benzo(a)pyrene in edible oil |
| CN105203373A (en) * | 2015-09-10 | 2015-12-30 | 上海安谱实验科技股份有限公司 | Method for simply, fast, efficiently and stably testing benzopyrene in food |
| CN105223301A (en) * | 2015-09-23 | 2016-01-06 | 成都艾比科生物科技有限公司 | A kind of method for measuring benzopyrene content in vegetable oil |
| CN105954369B (en) * | 2016-04-19 | 2018-04-06 | 中华人民共和国吉林出入境检验检疫局 | Benzo in a kind of homogeneous liquid-liquid extraction Water By High Performance Liquid of ionic liquid（α）The analysis method of pyrene |
| CN105954369A (en) * | 2016-04-19 | 2016-09-21 | 中华人民共和国吉林出入境检验检疫局 | Analysis method for determining benzo(alpha)pyrene in water through ionic liquid homogeneous liquid-liquid extraction and high-performance liquid chromatography |
| CN105866288A (en) * | 2016-05-10 | 2016-08-17 | 芜湖雨耕山食品检测有限公司 | Method of utilizing high performance liquid chromatography to detect benzo (a) pyrene in edible oil |
| CN106053371A (en) * | 2016-05-17 | 2016-10-26 | 中国科学院青岛生物能源与过程研究所 | Method for rapidly detecting benzopyrene in plant oil |
| CN106053371B (en) * | 2016-05-17 | 2018-11-09 | 中国科学院青岛生物能源与过程研究所 | The rapid detection method of BaP in one vegetable oil |
| CN108645689A (en) * | 2018-04-28 | 2018-10-12 | 山东省食品药品检验研究院 | A kind of device and method for BaP detection pre-treatment |
| CN108645689B (en) * | 2018-04-28 | 2023-12-08 | 山东省食品药品检验研究院 | Device and method for benzopyrene detection pretreatment |
| CN110609096A (en) * | 2019-09-02 | 2019-12-24 | 宁波中盛产品检测有限公司 | Rapid extraction and purification method for 4 polycyclic aromatic hydrocarbon compounds in edible oil and detection application thereof |
| CN110609096B (en) * | 2019-09-02 | 2022-03-11 | 宁波中盛产品检测有限公司 | Rapid extraction and purification method for 4 polycyclic aromatic hydrocarbon compounds in edible oil and detection application thereof |
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