CN102721763B - Method for detecting chloropropanol ester in oil by high performance liquid chromatography - Google Patents
Method for detecting chloropropanol ester in oil by high performance liquid chromatography Download PDFInfo
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- CN102721763B CN102721763B CN 201210222201 CN201210222201A CN102721763B CN 102721763 B CN102721763 B CN 102721763B CN 201210222201 CN201210222201 CN 201210222201 CN 201210222201 A CN201210222201 A CN 201210222201A CN 102721763 B CN102721763 B CN 102721763B
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- propylene chlorohydrin
- chlorohydrin ester
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Abstract
The invention provides a method for detecting chloropropanol ester in oil by high performance liquid chromatography. The method is characterized by comprising the following steps of: removing triglyceride and polar components from the oil, and detecting the treated oil by the high performance liquid chromatography, wherein the chromatographic condition is that a normal phase silica gel chromatographic column is used; normal hexane and isopropyl alcohol are respectively used as a flow phase A and a flow phase B; isocratic elution is performed at the flow speed of 0.5 mL/min; an evaporation dispersion detector is used for performing detection; and the volume ratio of the flow phase A to the flow phase B is 9: 1. The method has the advantages that the chloropropanol ester content in the oil can be detected by the simple method.
Description
Technical field
The present invention relates to a kind of propylene chlorohydrin ester detection method, relate in particular to the method that a kind of high performance liquid chromatography detects propylene chlorohydrin ester in the grease.
Background technology
The detection method of the propylene chlorohydrin ester that the present invention relates to is the detection for grease propylene chlorohydrin ester.The propylene chlorohydrin ester is grease and contains the accessory substance that fatty foods forms in hot procedure, is considered at present one of potential food safety hazard factor.
The method of propylene chlorohydrin ester mainly contains GC-MS, LC-MS, LC-MS/MS etc. in the detection grease of bibliographical information at present.The detection sensitivity of these methods is all higher, but its required instrument is expensive, requires the professional to operate, and maintenance and use cost are high, therefore only is fit to the large-scale experiment chamber and uses.
Moravcova has reported a kind of method (Moravcova that detects propylene chlorohydrin ester in the grease, E.and L.Vaclavik, et al.Novel approaches to analysis of 3-chloropropane-1,2-diol esters in vegetable oils.Analytical and Bioanalytical Chemistry.2012.), its concrete operations are to be loaded to silicagel column and (to fill required silica gel with normal hexane/diethyl ether (96: 4 having added the oil sample of deuterium for internal standard compound, v/v) potpourri swelling), with 30 ml n-hexanes/diethyl ether (96: 4, v/v) potpourri isocratic elution, elution speed is 0.8 ml/min, discard 0～5 milliliter part, collect 5～25 milliliters part, after the rotary evaporation desolventizing, residue dissolves with methyl alcohol, prepares to carry out U-HPLC-MS and analyzes.Weak point be operating cycle of whole silica gel column chromatography more than 1 hour, this is unfavorable for carrying out that oil sample in batches processes; Simultaneously, having relatively high expectations of U-HPLC-MS system flow phase it is reported, at present domestic chromatographically pure reagent is except methyl alcohol, acetonitrile, and all the other are not suitable for this cover system, and the cost that oil sample detects is higher.
The inventive method with organic solvent except triglyceride and polar compound in the degrease, then adopt high performance liquid chromatography to detect, wherein, chromatographic condition is: use the normal phase silica gel chromatography post, respectively take normal hexane and isopropyl alcohol as mobile phase A and Mobile phase B, with flow velocity 0.5mL/min isocratic elution, evaporative light-scattering detector detects, and the volume ratio of mobile phase A and Mobile phase B is 9: 1.
Summary of the invention
The present invention overcomes shortcoming of the prior art, and the propylene chlorohydrin ester that a kind of oil sample pre-treatment is simple, detection sensitivity is high and the method application is good detection method is provided, and at many analysis fields such as food, medicine, environment higher using value is arranged.
In order to solve the problem of above-mentioned technology, the present invention is achieved by the following technical solutions: a kind of high performance liquid chromatography detects the method for propylene chlorohydrin ester in the grease, it is characterized in that, concrete steps are:
The first step: grease is heated to liquid condition, and triglyceride is removed in pre-service;
Second step: the sample of the removal triglyceride of first step gained is processed, removed polar compound, with the acetonitrile dissolving, obtain sample solution;
The 3rd step: measure when daily dilution in acetonitrile preparation propylene chlorohydrin ester standard solution, its concentration is C
S, obtaining standard solution with 0.2 μ m aperture filtering membrane filtration, high performance liquid chromatography detects delivery time and the peak area A thereof that obtains the propylene chlorohydrin ester
S, chromatographic condition is: use the normal phase silica gel chromatography post, take normal hexane and isopropyl alcohol as mobile phase A and Mobile phase B, with flow velocity 0.5mL/min isocratic elution, evaporative light-scattering detector detects respectively, and the volume ratio of mobile phase A and Mobile phase B is 9: 1;
The 4th step: the sample solution of second step gained is obtained sample solution with 0.2 μ m aperture filtering membrane filtration, adopt the chromatographic condition test sample solution identical with the 3rd step, obtain the peak area A corresponding with the delivery time of propylene chlorohydrin ester
i, be calculated as follows the concentration C of propylene chlorohydrin ester in the grease
i:
C
i＝C
S·(A
i/A
S)。
The concrete steps of in the described first step grease pre-service being removed sweet three esters are: add the acetonitrile of 2 times of volumes in the grease sample, vortex oscillation 30s with the centrifugal 10min of rotating speed 10000r/min, gets supernatant, in 50 ℃ of rotation evaporates to dryness.
In the described second step sample of the removal triglyceride of first step gained being processed the concrete steps of removing polar compound is: the normal hexane that adds 2 times of volumes in the sample of the removal triglyceride of first step gained, vortex oscillation 30s, with the centrifugal 10min of rotating speed 10000r/min, get supernatant, in room temperature rotation evaporate to dryness, the gained dry residue dissolves with acetonitrile, obtains sample solution.
Compared with prior art, the invention has the advantages that: the content that can detect by simple method propylene chlorohydrin ester in the grease.
Embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1
A kind of high performance liquid chromatography detects the method for propylene chlorohydrin ester in the grease:
The first step: will fry the heating of the degree of 28 behind 30h palm oil samples, and make to be liquid condition, and add the acetonitrile of 2 times of volumes, vortex oscillation 30s with the centrifugal 10min of rotating speed 10000r/min, gets supernatant, in 50 ℃ of rotation evaporates to dryness;
Second step: add the normal hexane of 2 times of volumes in the dry residue, vortex oscillation 30s with the centrifugal 10min of rotating speed 10000r/min, gets supernatant, and in room temperature rotation evaporate to dryness, the gained dry residue dissolves with acetonitrile, obtains sample solution;
The 3rd step: with dilution in acetonitrile preparation propylene chlorohydrin ester standard solution, its concentration C
SBe 0.156mg/mL, filter with 0.2 μ m aperture filtering membrane and obtain standard solution, it is 5.26min and peak area A that high performance liquid chromatography detects the delivery time that obtains the propylene chlorohydrin ester
SBe 1962690mVs, chromatographic condition is: use Hedera Si chromatographic column, (Ф 4.6 * 200mm, 3 μ m, Hanbon Sci.﹠amp; Tech.), sample size 5 μ L, take normal hexane and isopropyl alcohol as mobile phase A and Mobile phase B, with flow velocity 0.5mL/min isocratic elution, evaporative light-scattering detector detects respectively, and the volume ratio of mobile phase A and Mobile phase B is 9: 1;
The 4th step: the sample solution of second step gained is obtained sample solution with 0.2 μ m aperture filtering membrane filtration, adopt the chromatographic condition test sample solution identical with the 3rd step, obtain the peak area A corresponding with the delivery time of propylene chlorohydrin ester
iBe 10749041mVs, be calculated as follows the concentration C of propylene chlorohydrin ester in the grease
i:
C
i＝C
S·(A
i/A
S)＝0.85mg/mL。
Embodiment 2
Another kind of high performance liquid chromatography detects the method for propylene chlorohydrin ester in the grease:
The first step: in adding the acetonitrile that adds 2 times of volumes in 3% sodium chloride, the corn oil sample of 5% water behind 240 ℃ of heating 3h, vortex oscillation 30s with the centrifugal 10min of rotating speed 10000r/min, gets supernatant, in 50 ℃ of rotation evaporates to dryness;
Second step: add the normal hexane of 2 times of volumes in the dry residue, vortex oscillation 30s with the centrifugal 10min of rotating speed 10000r/min, gets supernatant, and in room temperature rotation evaporate to dryness, the gained dry residue dissolves with acetonitrile, obtains sample solution;
The 3rd step: with dilution in acetonitrile preparation propylene chlorohydrin ester standard solution, its concentration C
SBe 0.208mg/mL, filter with 0.2 μ m aperture filtering membrane and obtain standard solution, it is 5.26min and peak area A that high performance liquid chromatography detects the delivery time that obtains the propylene chlorohydrin ester
SBe 3504038mVs, chromatographic condition is: use Hedera Si chromatographic column, (Ф 4.6 * 200mm, 3 μ m, Hanbon Sci.﹠amp; Tech.), sample size 5 μ L, take normal hexane and isopropyl alcohol as mobile phase A and Mobile phase B, with flow velocity 0.5mL/min isocratic elution, evaporative light-scattering detector detects respectively, and the volume ratio of mobile phase A and Mobile phase B is 9: 1;
The 4th step: the sample solution of second step gained is obtained sample solution with 0.2 μ m aperture filtering membrane filtration, adopt the chromatographic condition test sample solution identical with the 3rd step, obtain the peak area A corresponding with the delivery time of propylene chlorohydrin ester
iBe 1008579mVs, be calculated as follows the concentration C of propylene chlorohydrin ester in the grease
i:
C
i＝C
S·(A
i/A
S)＝0.06mg/mL。
Claims (3)
1. a high performance liquid chromatography detects the method for propylene chlorohydrin ester in the grease, it is characterized in that, concrete steps are:
The first step: grease is heated to liquid condition, and triglyceride is removed in pre-service;
Second step: the sample of the removal triglyceride of first step gained is processed, removed polar compound, with the acetonitrile dissolving, obtain sample solution;
The 3rd step: measure when daily dilution in acetonitrile preparation propylene chlorohydrin ester standard solution, its concentration is C
S, obtaining standard solution with 0.2 μ m aperture filtering membrane filtration, high performance liquid chromatography detects delivery time and the peak area A thereof that obtains the propylene chlorohydrin ester
S, chromatographic condition is: use specification to be Φ 4.6 * 200mm, the Hedera Si chromatographic column of 3 μ m, respectively take normal hexane and isopropyl alcohol as mobile phase A and Mobile phase B, with flow velocity 0.5mL/min isocratic elution, evaporative light-scattering detector detects, and the volume ratio of mobile phase A and Mobile phase B is 9: 1;
The 4th step: the sample solution of second step gained is obtained sample solution with 0.2 μ m aperture filtering membrane filtration, adopt the chromatographic condition test sample solution identical with the 3rd step, obtain the peak area A corresponding with the delivery time of propylene chlorohydrin ester
i, be calculated as follows the concentration C of propylene chlorohydrin ester in the grease
i:
C
i＝C
S·(A
i/A
S)。
2. the method for propylene chlorohydrin ester in the detection grease as claimed in claim 1, it is characterized in that, the concrete steps of in the described first step grease pre-service being removed sweet three esters are: the acetonitrile that adds 2 times of volumes in the grease sample, vortex oscillation 30s, with the centrifugal 10min of rotating speed 10000r/min, get supernatant, in 50 ℃ of rotation evaporates to dryness.
3. the method for propylene chlorohydrin ester in the detection grease as claimed in claim 1, it is characterized in that, in the described second step sample of the removal triglyceride of first step gained being processed the concrete steps of removing polar compound is: the normal hexane that adds 2 times of volumes in the sample of the removal triglyceride of first step gained, vortex oscillation 30s, with the centrifugal 10min of rotating speed 10000r/min, get supernatant, in room temperature rotation evaporate to dryness, the gained dry residue dissolves with acetonitrile, obtains sample solution.
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|---|---|---|---|
| CN 201210222201 CN102721763B (en) | 2012-07-02 | 2012-07-02 | Method for detecting chloropropanol ester in oil by high performance liquid chromatography |
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| CN102721763B true CN102721763B (en) | 2013-10-16 |
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| CN103245752B (en) * | 2013-04-15 | 2015-08-12 | 福建省疾病预防控制中心 | A kind of method detecting fatty acid chloropropanol ester pH-titration in food |
| CN106501390A (en) * | 2016-09-26 | 2017-03-15 | 广东出入境检验检疫局检验检疫技术中心 | A kind of at the same detect food in 3 chloropropanol esters and ethylene oxidic ester method |
| CN111879770B (en) * | 2020-09-28 | 2020-12-11 | 广州智汇生物科技有限公司 | Method for detecting hair water in fermented soy product |
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| CN102492741B (en) * | 2011-12-22 | 2014-04-09 | 江南大学 | Synthesizing method of chloropropanol ester |
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Effective date of registration: 20160830 Address after: 201506 No. 6505, Ting Wei Road, Jinshan Industrial District, Shanghai Patentee after: Shanghai Rong's health industry Limited by Share Ltd Address before: Food College of Jiangnan University No. 1800 214122 Jiangsu city of Wuxi Province Li Lake Avenue Patentee before: Jiangnan University |
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