目的:建立QuEChERS技术结合气相色谱-串联质谱(GC-MS/MS)同时检测山药中50种农药的检测方法,并对30批来自市场的山药进行初步筛查。方法:山药样品加水经1%醋酸乙腈提取,依次经QuEChERS提取剂和QuEChERS净化剂盐析净化,提取液经浓缩后,加入内标环氧七氯B,采用GC-MS/MS进行检测分析。结果:50种农药质量浓度在0.002~0.2 mg·L-1范围内线性关系良好,相关系数(r)均大于0.99;3个添加水平的平均回收率为71.2%~104.1%,87%的农药RSD小于5.0%;50种农药的检测下限为0.2~3.4 μg·kg-1;对30批山药样品进行检测,共检出6种农药,其中二嗪磷检出率高达73.3%。结论:本方法简便、灵敏、准确,可用于山药中多种农药残留的快速筛查与检测,为山药的种植生产和质量管控提供技术支撑。
Objective: To establish a analysis method of QuEChERS technology combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) to detect 50 pesticide residues in Chinese Yam, and to screen 30 batches of Yam samples from markets. Methods: Samples weretreated with water and extracted with acetonitrile, and the QuEChERS package was used for salting out. After the extraction solution was concentrated, internal standard heptachlor-epoxide B was added, and GC-MS/MS was used for detection and analysis. Results: The linear ranges of 50 pesticides were from 0. 002 to 0.2 mg·L-1, with the correlation coefficient (r) greater than 0.99. The average recoveries were ranged from 71.2% to 104.1% of three concentration added standard, and 87% of the pesticides with the RSDs were less than 5.0%. Detection limits of 50 pesticides were from 0.2 to 3.4 μg·kg-1. Thirty batches of Chinese Yam samples were tested and six pesticides were detected. The detection rate of diazinon was 73.3%. Conclusion: This method is simple, sensitive and accurate, which can be used for rapid screening and detection of various pesticide residues in Chinese Yam, and can provide technical support for the cultivation, production and quality control of Chinese Yam.
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