Method for rapidly determining acrylamide in vegetable oil by QuEChERS-LC-MS/MS

Abstract

The invention discloses a method for rapidly determining acrylamide in vegetable oil by QuEChERS-LC-MS / MS. The method comprises: extracting acrylamide in the oil sample by acetonitrile; and after freezing and degreasing, purifying the supernatant by MgSO4, C18, PSA and GCB adsorbents, separating by a C18 chromatographic column, carrying out gradient elution by adopting a methanol -0.1% formic acidaqueous solution mobile phase, detecting by adopting a triple quadrupole mass spectrometry electrospray multi-reaction monitoring mode (MRM), and quantifying by adopting an internal standard method.The acrylamide has a good linear relationship in a concentration range of 1-500 ng / mL, and the correlation coefficient is greater than 0.997. The detection limit of the method is 2 [mu]g / kg, and the quantification limit is 5 [mu]g / kg. The adding standard recovery rate is 96.4%-108%, and the relative standard deviation is less than 7.74%. The method has the advantages of simple and efficient pretreatment operation, direct on-machine determination without concentration, good recovery rate, high sensitivity, and accurate qualitative and quantitative determination.

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...

AI Technical Summary

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

Images