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改进的QuEChERS结合HPLC-MS/MS法同时测定中药水蛭中26种农药残留量

Simultaneous Determination of 26 Pesticide Residues in Traditional Chinese Medicinal Leeches by Modified QuEChERS Coupled with HPLC-MS/MS.

作者信息

Zhou Ying, Yu Yahui, Huang Qian, Zheng Huixin, Zhan Ruyi, Chen Luting, Meng Xingang

机构信息

College of Biological and Environmental Engineering, Jingdezhen University, Jingdezhen City 334000, Jiangxi Province, P.R. China.

Jingdezhen Nursing School, Jingdezhen 333000, P.R. China.

出版信息

ACS Omega. 2023 Mar 22;8(13):12404-12410. doi: 10.1021/acsomega.3c00217. eCollection 2023 Apr 4.

Abstract

A Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) pretreatment technique combined with HPLC-MS/MS was established to detect 26 pesticides in traditional Chinese medicinal leeches. The sample was extracted by acetonitrile solution with sodium acetate-0.1% (v/v) acetic acid as a buffer system, then cleaned up by a mixture of 750 mg of MgSO, 150 mg of C, and 150 mg of PSA, separated by an ACQUITY BEH C column, and determined in the dynamic multiple reaction mode. Under the optimized conditions, the peak areas of the 26 pesticides in leeches showed good linearity ( > 0.99) between their mass concentrations from 1 to 100 μg/L. At the spike levels of 10, 20, and 100 μg/kg, the recoveries of 26 pesticides in leeches were 72.9-101.6% with an RSD of 1.1-12.8%, an LOQ of 10 μg/kg, and an LOD of 0.1-5.4 μg/kg. This method is easy, rapid, sensitive, and practical and meets the requirements of pesticide residue detection standards.

摘要

建立了一种快速、简便、廉价、高效、耐用且安全(QuEChERS)的预处理技术与高效液相色谱-串联质谱联用方法,用于检测传统中药水蛭中的26种农药。样品用乙腈溶液提取,以醋酸钠-0.1%(v/v)乙酸为缓冲体系,然后用750 mg硫酸镁、150 mg C和150 mg PSA的混合物净化,经ACQUITY BEH C柱分离,采用动态多反应监测模式测定。在优化条件下,水蛭中26种农药的峰面积在其质量浓度1至100 μg/L之间呈现良好的线性关系(r>0.99)。在10、20和100 μg/kg的加标水平下,水蛭中26种农药的回收率为72.9-101.6%,相对标准偏差为1.1-12.8%,定量限为10 μg/kg,检测限为0.1-5.4 μg/kg。该方法简便、快速、灵敏、实用,符合农药残留检测标准要求。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/bf03/10077569/5e4cd91dc843/ao3c00217_0002.jpg

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