广陈皮中71种禁限用农药残留测定分析

目的：建立广陈皮中禁限用化学农药多残留的检测方法。方法：以乙腈为溶剂，高速匀浆提取，经HLB SPE小柱及改良的QuEChERs填料净化。检测方法：气相色谱-串联质谱法，采用DB-17MS弹性石英毛细管柱（30 m×0.25 mm×0.25 μm），电子轰击电离源（EI）；液相色谱-串联质谱法，采用Kinetex C₁₈色谱柱（100 mm×2.1 mm，2.6 μm），以0.1%甲酸溶液（含5 mmol·L^-1甲酸铵）溶液和95%乙腈（含5 mmol·L^-1甲酸铵和0.1%甲酸）溶液为流动相进行梯度洗脱，电喷雾电离源（ESI），正离子模式下多反应监测（MRM）。结果：71种待测指标成分线性关系良好，相关系数均大于0.99，三水平加样回收率全部指标在71.8%～116.8%，RSD为0.90%～14.1%，符合多农残的痕量分析检测要求。结论：61批样品中共检出禁限用农药18种，合格率60.6%。该方法有针对性地对广陈皮中71种禁限用农药残留进行快速筛查与准确检测，适用于对中药广陈皮的日常监控，同时为基质类似中药的农药残留方法提供借鉴。

Objective: To establish a method for the determination of forbidden and restricted pesticide residues in Citri reticulatae ‘Chachi’. Methods: The samples were extracted with acetonitrile by high speed homogenizer,and purified by HLB SPE or modified QuEChERs. GC-MS/MS analysis was performed on a DB-17MS (30 m×0.25 mm×0.25 μm) capillary column with electron impact (EI) source. An LC-MS/MS analysis was performed on a Kinetex C₁₈ column (100 mm×2.1 mm,2.6 μm) with gradient elution of 0.1% formic acid (containing 5 mmol·L^-1 ammonium formate) and 95% acetonitrile (containing 5 mmol·L^-1 ammonium formate and 0.1% formic acid). Electrospray ionization(ESI) source was applied by positive ionization in multiple reaction monitoring(MRM) modes. Results: The calibration curves of 71 targets showed good linearity with correlation coefficients of above 0.99. The average recoveries at three levels for all target were in the range of 71.8%-116.8%,with RSDs of 0.90%-14.1%,met with the requirements of multi-pesticides trace analysis. Conclusion: There were 18 pesticides detected in all 61 samples,with total acceptance rate of 60.6%. The detecting method covers 71 kinds of forbidden and restricted pesticides,which is suitable for the rapid screening and accurately determination of pesticides residues for routine monitoring and safely control in Citri reticulatae ‘Chachi’ plant. The method can provide reference for multi-pesticides residues of other similar matrix of medicinal plants.

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