超高效液相色谱-串联质谱法测定中药材中三唑类杀菌剂及三嗪类除草剂的残留量

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定甘草、西洋参、三七、人参、丹参5种中药材中10种三唑类杀菌剂、18种三嗪类除草剂(包括有毒代谢物)残留量的分析方法。采用QuEChERS前处理方法,样品经1%(v/v)醋酸乙腈提取,乙二胺-N-丙基硅烷(PSA)净化处理,以Shim-pack XR-ODSII(75 mm×2.0 mm)为色谱柱,0.05%(v/v)甲酸溶液-乙腈为流动相梯度洗脱,在多反应监测(MRM)模式下测定。25种农药及其3种有毒代谢物的定量限(S/N≥10)为0.20～5.52 μg/kg;检出限(S/N≥3)为0.10～2.57 μg/kg;在各自的考察浓度范围内线性关系良好(r≥0.999);在0.20～55.2 μg/kg添加水平内,平均加标回收率为70.6%～125.7%,RSD为0.7%～14.2%。该方法样品前处理简单、快速、灵敏,可用于中药材中三唑类杀菌剂和三嗪类除草剂农药残留量的快速筛查。

Determination of triazole fungicide and triazine herbicide residues in Chinese herbs by ultra-performance liquid chromatography-tandem mass spectrometry

A method using QuEChERS clean-up followed by UPLC-MS/MS has been established for the quantitative determination of the residues of 10 triazole fungicides and 18 triazine herbicides in Chinese herbs including Radix Glycyrrhizae, Radix Panacis Quinquefolii, Salvia miltiorrhiza, Radix Notoginseng and Panax ginseng C. The pesticide residues were extracted from the samples by acetonitrile containing 1%(v/v) acetic acid, cleaned-up with primary secondary amine (PSA) and then analyzed using UPLC-MS/MS in multiple reaction monitoring (MRM) mode with positive electrospray ionization. The analytical column was Shim-pack XR-ODSII(75 mm×2.0 mm) and the mobile phases were water containing 0.05% (v/v) formic acid and acetonitrile in gradient elution. The limits of quantification (S/N≥10) of the 28 pesticides were 0.20-5.52 μg/kg and the limits of detection (S/N≥3) were 0.10-2.57 μg/kg. All of the pesticides had good linear responses with r≥0.999 and the average recoveries of the pesticides spiked in the Chinese herbs ranged from 70.6%-125.7% with the RSDs of 0.7%-14.2%. The results demonstrated that the method is simple, fast and sensitive to meet the requirements for the triazole fungicide and triazine herbicide residues and can be used for the analysis of the 28 pesticides in the above five Chinese herbs.