目的 建立QuEChERS-反相高效液相色谱-串联质谱法测定麦冬药材中多效唑、烯效唑的农药残留的方法。方法 采用Thermo BDS Hypersil C₁₈色谱柱（100 mm×4.6 mm，2.4 mm）；流动相：0.1%甲酸的0.005 mol/L醋酸铵溶液-乙腈（25：75）；柱温：25℃；体积流量：0.3 mL/min；进样量：10 μL；检测波长：223 nm。采用电喷雾正离子模式进行多反应监测，喷雾电压：5 000 V，毛细管温度：450℃，鞘气：206 kPa，辅助气：15 mL/min。结果 多效唑、烯效唑浓度在1.0~100 ng/mL线性关系良好。多效唑、烯效唑的检出限分别为0.05、0.01 ng/mL，定量限分别为0.22、0.03 ng/mL。多效唑、烯效唑的平均回收率分别为94.7%、85.5%，RSD值分别为5.3%、4.1%。在33个实际样品中有31个样品检出多效唑残留，检出率为94%，残留量为0.02~2.08 mg/kg；有9个样品检出烯效唑残留，检出率为27%，残留量为0.02~0.13 mg/kg。结论 本方法可快速、简便、准确地测定麦冬药材中的多效唑、烯效唑残留量。

Objective To establish a QuEChERS-HPLC-MS/MS method for the determination of pesticide residues of paclobutrazol and uniconazole in Ophiopogonis Radix.Methods The separation was carried out on Thermo BDS Hypersil C₁₈ (100 mm×4.6 mm, 2.4 mm). The mobile phase was consisted of 0.005 mol/L ammonium acetate solution of 0.1% formic acid - acetonitrile (25:75). The column temperature was set at 25 ℃, flow rate was 0.3 mL/min, and volume of injection was 10 μL. The detective wavelength was set at 223 nm. Electrospray positive ion mode was used for multi reaction monitoring, the spray voltage was set at 5 000 V, and the capillary temperature was set at 450 ℃. Sheath gas was 206 kPa and the auxiliary gas was 15 mL/min.Results The linear ranges of paclobutrazol and uniconazole were 1.0 — 100 ng/mL. The detection limits of paclobutrazol and uniconazole were 0.05, 0.01 ng/mL, and quantitative limits were 0.22, 0.03 ng/mL, respectively. The average recoveries of paclobutrazol and uniconazole were 94.7% and 85.5% with RSD of 5.3% and 4.1%, respectively. In the 33 actual samples, 31 samples were detected with the paclobutrazol detection rate of 94% and with the residual amount of 0.02 — 2.08 mg/kg. In 9 samples, the uniconazole detection rate was 27%, and the residues were 0.02 — 0.13 mg/kg.Conclusion The method is rapid, simple, and accurate for the determination of paclobutrazol and uniconazole residues in Ophiopogonis Radix.

中国医学科学院医学与健康科技创新工程协同创新团队项目（2017-12M-3-013）