Improved quechers-lc-ms/ms method for rapid determination of acrylamide in vegetable oil

A technology for rapid determination of acrylamide, which is applied in the field of food inspection, can solve the problems of lack of in-depth research on acrylamide detection, complicated derivation process, and inapplicability of acrylamide, etc., to overcome the problem of easy loss, simple and efficient operation, and good linear relationship Effect

Active Publication Date: 2022-03-04
SHANDONG INST FOR FOOD & DRUG CONTROL
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  • Application Information

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Problems solved by technology

At present, the commonly used pretreatment methods for the detection of acrylamide in food include solid-phase extraction column method, matrix-dispersed solid-phase extraction, liquid-liquid extraction, and molecular imprinting. Poor, low sample recovery and other disadvantages
The current detection standards for acrylamide in food in my country mainly include GB 5009.204-2014 (HPLC-MS / MS method and GC-MS method) and SN / T 2096-2008 (GC-MS), except that gas chromatography-mass spectrometry requires a derivation process In addition to the disadvantages of complexity, the purification method adopts the classic pretreatment method of acrylamide, that is, the dual solid-phase extraction column purification method after water extraction, which has the disadvantages of complicated operation and low recovery rate, and the method is not suitable for the detection of acrylamide in vegetable oil.
[0005] The QuEChERS method was initially used as a relatively mature pretreatment method for the detection of pesticide residues. Due to its high efficiency, simplicity, and quickness, it has been gradually used for the purification of veterinary drug residues, toxins, and pollutants in various matrices, and the purification of pesticide residues, toxins, and polyphenols in vegetable oils. The detection of similar compounds and heterocyclic amines has been reported using optimized QuEChERS, but there is no in-depth study on the detection of acrylamide in vegetable oil. Amide and whether it adsorbs acrylamide is unknown, so whether it affects the detection results of acrylamide is also unknown. How to achieve the optimal detection of acrylamide in vegetable oil needs to be studied

Method used

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  • Improved quechers-lc-ms/ms method for rapid determination of acrylamide in vegetable oil
  • Improved quechers-lc-ms/ms method for rapid determination of acrylamide in vegetable oil
  • Improved quechers-lc-ms/ms method for rapid determination of acrylamide in vegetable oil

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Embodiment 1

[0040] 1 Instruments and reagents

[0041] TSQ Quantiva liquid chromatography-triple quadrupole tandem mass spectrometer, equipped with electrospray ion source, ThermoFisher Company of the United States; Sigma 3-18K high-speed refrigerated centrifuge, Sigma Company of Germany; ultrasonic cleaner, Ningbo Xinzhi Biotechnology Co., Ltd.; MS3 vortex mixer, IKA company, N-EVAP-45 position nitrogen blowing instrument, American Organomation company; SQP-electronic balance, Sartorius Scientific Instrument Co., Ltd.; ultrapure water, Mili-Q ultrapure water machine.

[0042] Acrylamide standard substance (purity ≥ 99%), German Dr company, 13C3-acrylamide isotope internal standard (purity ≥ 99%), German WITEGA company; Methanol, acetonitrile, cyclohexane, ethyl acetate (chromatographically pure), the United States Bruker company; Formic acid, ammonium acetate (chromatographically pure), U.S. Sigma-Aldrich company; Water is Milli-Q ultrapure water machine preparation; Nitrogen (>99.999%);...

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Abstract

The invention discloses a QuEChERS‑LC‑MS / MS method for quickly determining acrylamide in vegetable oil. The acrylamide in the oil sample is extracted with acetonitrile, and after freezing and degreasing, the supernatant is passed through MgSO 4 , C18, PSA and GCB adsorbents for purification, C18 chromatographic column separation, gradient elution with methanol-0.1% formic acid aqueous mobile phase, triple quadrupole mass spectrometry electrospray multiple reaction monitoring mode (MRM) detection, internal standard method for quantification . Acrylamide had a good linear relationship within the concentration range of 1-500 ng / mL, and the correlation coefficient was greater than 0.997. The detection limit of the method is 2 μg / kg, and the limit of quantification is 5 μg / kg. The recoveries of standard addition were between 96.4% and 108%, and the relative standard deviations were all less than 7.74%. The pretreatment operation of the invention is simple and efficient, and the method can be directly measured on a machine without concentration, and the method has good recovery rate, high sensitivity, and accurate qualitative and quantitative results.

Description

technical field [0001] The invention belongs to the field of food inspection, and in particular relates to an improved QuEChERS-LC-MS / MS method for rapidly determining acrylamide in vegetable oil. Background technique [0002] Acrylamide mainly exists in fried and over-baked foods. It is a Class 2A carcinogen and has various toxic and side effects on animals such as neurotoxicity, reproductive toxicity, mutagenicity and carcinogenicity. Organizations such as the World Health Organization (WHO) warn the public to pay attention to acrylamide in food, and call for measures to reduce the content of acrylamide in food to ensure food safety. After Swedish scientists discovered acrylamide in baked, fried and other foods for the first time, the pollution problem in its food began to attract people's attention. However, the Starbucks acrylamide cancer scandal in 2018 and the 2019 incidents of "Fengwei Cookies Containing Acrylamide" and "Muji Biscuits Cause Cancer" have once again br...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/7266G01N30/8679
Inventor张艳侠刘艳明孙珊珊祝建华赵慧男胡梅王明栋郑文静
OwnerSHANDONG INST FOR FOOD & DRUG CONTROL