Screening of pesticide residues in Traditional Chinese Medicines using modified QuEChERS sample preparation procedure and LC-MS/MS analysis
Screening of pesticide residues in Traditional Chinese Medicines using modified QuEChERS sample preparation procedure and LC-MS/MS analysis
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使用改进的 QuEChERS 样品制备程序和 LC-MS/MS 分析筛查中药中的农药残留
DOI：
10.1016/j.jchromb.2020.122224
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发表时间：
2020-09-01
影响因子：
3
通讯作者：
Dai, Xiao-Feng
中科院分区：
文献类型：
--
作者：
Li, Rui-Xing;Li, Min-Min;Dai, Xiao-Feng
建立了一种高效液相色谱-串联质谱（UHPLC-MS/MS）同时测定中药中108种农药残留的方法。在含0.75%（v/v）乙酸的乙腈中超声提取15 min，以MgSO 4和C18为分散固相萃取剂。该方法具有良好的线性关系（r（2）> 0.9901），选择性好，精密度和重复性好。超过92%的农药表现出高比率或回收率在70-120%的范围内。该方法显示出高灵敏度，在厚朴中的定量限在0.01-20 ng/mL范围内，在其他中药中为0.01-50 ng/mL。应用该方法对39个不同产地的真实的样品进行了分析，检出率为92.3%，其中3种中药共检出26种农药。在三分之一的样本中检测到四种以上的农药。其中，戊唑醇在三种中药中均检出，浓度为0.22-22.02 μ g/kg，低于GB 2763-2019中的规定（50 μ g/kg）。此外，麦冬中多效唑的检出率为100%，有9个样品的检出浓度超过了蔬菜最高残留限量标准（50微克/千克）。考虑到中国没有规定这三种中药的农药残留限量，我们建议加快制定适当的法规。
A robust and high-throughput method was developed for the determination of 108 pesticide residues in Traditional Chinese Medicines (TCMs) simultaneously using a combination of UHPLC-MS/MS analysis and the modified QuEChERS method. Extraction was carried out in acetonitrile containing 0.75% (v/v) acetic acid with ultrasonication for 15 min; MgSO4 and C18 were used as the dispersive-solid phase extraction sorbents. The method exhibited good linearity (r(2) > 0.9901), in addition to good selectivity, precision and repeatability. More than 92% of pesticides exhibited high rates or recovery in the 70-120% range. This method showed high sensitivity, with Limits of Quantitation in the 0.01-20 ng/mL range in Cortex Moutan, and 0.01-50 ng/mL in the other TCMs. The method was employed for the analysis of 39 real samples from different habitats, and pesticides were detected in 92.3% of the samples, with 26 pesticides being detected in these three TCMs. More than four pesticides were detected in a third of the samples. Among them, tebuconazole was detected in all the three TCMs with 0.22-22.02 mu g/kg concentration, which was lower than the provisions in GB 2763-2019 (50 mu g/kg). In addition, the paclobutrazol detection rate in Ophiopogon japonicus was 100%, and the detected concentrations of 9 samples exceeded the Maximum Residue Levels defined for vegetables (50 mu g/kg). Considering there are no regulations that govern the limits of pesticide residues in the three TCMs in China, we recommend the acceleration of efforts to introduce appropriate regulations.