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| Determination of 17 mycotoxins in ghee by QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry |
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| DOI：10.19902/j.cnki.zgyz.1003-7969.240245 |
| KeyWord:QuEChERS UPLC-MS/MS ghee mycotoxin |
| FundProject:中国检验检疫科学研究院基本科研业务费项目（2023JK001） |
| Author Name | Affiliation | | YAN Xiaoxian1,2, WU Xingqiang1, XIA Han1,2, TONG Kaixuan1,
CHANG Qiaoying1, FAN Chunlin1, ZHU Zhehui3, CHEN Hui1 | 1.Chinese Academy of Inspection and Quarantine, Beijing 100176, China
2.College of Chemistry and
Materials Science, Hebei University, Baoding 071002, Hebei, China
3.Xizang Autonomous Region
Product Quality Supervision and Inspection Institute, Lhasa 850000, China |
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| Abstract: |
| In order to provide technical support for the monitoring, prevention and control of the risk of mycotoxin contamination in ghee, a method for the determination of 17 mycotoxins in ghee by QuEChERS technique combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The ghee sample was extracted with 3% formic acid in water and 3% formic acid in acetonitrile in a stepwise manner, and then salted with MgSO4 and NaCl. After centrifugation at 0 ℃ and defatting with n-hexane, the extract was purified with N-propylethylenediamine (PSA) and octadecylsilyl silica gel (C18) to obtain the test sample. The test sample was then analyzed on an ACQUITY UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) column to achieve the separation, and detected in multiple reaction monitoring (MRM) mode and quantified by standard method with matrix matching curve external. The results showed that the 17 mycotoxins demonstrated good linearity in the corresponded mass concentration ranges with the coefficients of determination (R2) greater than 0.999 1. The limits of detection (LOD) and the limits of quantification (LOQ) of the method were in the range of 0.15-3.00 μg/kg and 0.50-10.00 μg/kg, respectively. The recoveries of the 17 mycotoxins ranged from 72.3% to 112.2% at 1, 2 and 10 times LOQ spiked levels with relative standard deviations (RSD) less than 8.0%. Twenty batches of ghee samples were analyzed and tested by this method, and fumonisin B2 was detected in three batches, while T-2 toxin was detected in two batches. In summary, the method is sensitive, accurate, and effective for routine monitoring of mycotoxins in ghee. |
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