1. 安徽省药品审评查验中心，合肥 230051； 2. 合肥市食品药品检验中心，合肥 230088
Determination of 53 prohibited pesticide residues in Gastrodia elata by chromatography-tandem mass spectrometry
LUO Jingjing1, CHENG Qingbing2, JIN Fenghua2, WANG Wei2
1. Anhui center for drug certification and inspection, Hefei 230051, China; 2. Hefei Institute for Food and Drug Control, Hefei 230088, China
摘要：建立超高效液相色谱-串联质谱联用（UPLC-MS/MS）及气相色谱-串联质谱联用（GC-MS/MS）法测定天麻中 53 种禁用农药残留。采用乙腈直接提取和基于 QuEChERS 原则的固相萃取法对样品进行处理。UPLC-MS/MS法采用电喷雾离子源，正离子模式下多反应监测，色谱峰面积外标法定量；GC-MS/MS 法采用电子轰击离子源，色谱峰面积内标法定量。 53 种农药的质量浓度在一定范围内与响应值线性关系良好，相关系数均大于 0.990，检出限为0.001～0.005 mg/kg，定量限为 0.002～0.01 mg/kg。样品平均回收率为 71.4%～118.2%，测定结果的相对标准偏差为1.4%～6.3%（n=6）。该方法能快速、有效地检测天麻中的禁用农药残留量，可用于天麻质量评价。
Abstract：Ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) were established for the determination of 53 prohibited pesticide residues in Gastrodia elata. The samples were treated with acetonitrile extraction and solid phase extraction based on QuEChERS principle. Electric spray ion source and multi reaction monitoring in positive ion mode was used for UPLC- MS/MS, and chromatographic peak area external standard method was used for quantitative analysis. Electron bombardment ion source was used for GC-MS/MS, and chromatographic peak area internal standard method was used for quantitative analysis. The mass concentration of 53 pesticides had a good linear relationship with the response values in the certain range, the correlation coefficients were all more than 0.990, the detection limits were 0.001-0.005 mg/kg, and the quantitative limits were 0.002-0.01 mg/kg. The average recoveries were 71.4%-118.2%, and the relative standard deviation of the determination results were 1.4%-6.3%(n=6). The method can quickly and effectively detect the prohibited pesticide residues in Gastrodia elata, and it can be used for quality evaluation of Gastrodia elata.
Keywords：UPLC-MS/MS; GC-MS/MS; Gastrodia elata; prohibited pesticide residues
LUO Jingjing，CHENG Qingbing，JIN Fenghua，et al. Determination of 53 prohibited pesticide residues in Gastrodia elata bychromatography-tandem mass spectrometry[J]. Chemical Analysis and Meterage，2023，32(10)：49.