超高效液相色谱-串联质谱法测定白术中34种禁限用农药残留

Determination of 34 prohibited and restricted pesticide residues in Atractylodes by ultra-performance liquid chromatography-tandem mass spectrometry

目的建立白术34种禁限用农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,对21批市售白术进行检测,初步调查市售白术农药残留情况。方法样品用纯乙腈提取,提取液经Waters-HLB 3cc(60 mg)固相萃取柱净化后,采用Waters-C_(18)色谱柱分离,流动相为0.1%甲酸水(含10 mmol/L甲酸铵)-乙腈,梯度洗脱,根据保留时间在多反应监测正离子模式下,以外标法定量分析。结果各成分在各自质量浓度范围内线性关系良好,r均大于0.9980。检测限为0.8~4.0μg/kg,定量限为2.0~10.0μg/kg。平均回收率为74.1%~97.4%,RSD为0.6%~6.4%(n=9)。21批白术样品中共有13批样品检出7种农药残留。结论本方法操作简单、定量准确,具有较高的回收率和良好的重复性,适用于白术中禁限用农药多残留检测。

Objective To establish an ultra-performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)method for the detection of 34 prohibited and restricted pesticide residues in Atractylodes,and 21 batches of commercially available Atractylodes were detected to preliminarily investigate the pesticide residues in commercial Atractylodes.Methods The samples were extracted with pure acetonitrile,the extracts were purified by Waters-HLB 3cc(60 mg)solid phase extraction column,separated by Waters-C_(18) column,0.1%formic acid water(containing 10 mmol/L ammonium formate)and acetonitrile were used as mobile phases(gradient elution),and quantitatively analyzed by external standard method in multi-reaction monitoring positive ion mode according to the retention time.Results The linear relationship of each component was good in their respective concentration ranges,the correlation coefficients were all greater than 0.9980.The limits of detection were within 0.8-4.0μg/kg,and the limits of quantification were within 2.0-10.0μg/kg.The average recovery rate was 74.1%-97.4%,and RSD was 0.6%-6.4%(n=9).Seven pesticide residues were found in 13 batches of 21 Atractylodes macrocephalus samples.Conclusion This method is simple to operate,accurate in quantification,has high recovery rate and good repeatability,and is suitable for the detection of multiple residues of prohibited and restricted pesticides in Atractylodes.