高效液相色谱-串联质谱法测定陈皮中7种新烟碱类农药残留

Determination of 7 kinds of neonicotinoid pesticide residues in pericarpium citri reticulatae by high performance liquid chromatography- tandem mass spectrometry

中文关键词:  陈皮  新烟碱类农药  高效液相色谱-串联质谱法

英文关键词:pericarpium citri reticulatea  neonicotinoid pesticides  high performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定陈皮中噻虫嗪、噻虫胺、噻虫啉、呋虫胺、氯噻啉、吡虫啉、啶虫脒7种新烟碱类农药的分析方法。方法 陈皮中的7种新烟碱类农药经乙腈提取, 乙二胺-N-丙基硅烷化硅胶(primary secondary amine, PSA)吸附剂净化后, 经色谱柱Shim-pack XR-ODS (100 mm×2.0 mm, 3 μm)分离, 采用高效液相色谱-串联质谱法测定, 外标法定量。结果 方法的检出限为0.1~2 μg/kg, 在0.5~50 μg/L测定范围内有良好的线性关系(r2＞0.9995), 在所添加3个水平浓度下, 方法的回收率在71.0%~117.0%, 相对标准偏差为1.8%~11.2%。结论 该方法准确、简单快速, 能满足农药残留检测方法的要求。

英文摘要:

      Objective To establish a method for simultaneous determination of 7 kinds of neonicotinoid pesticides (thiamethoxam, clothianidin, thiacloprid, dinotefuran, imidaclothiz, imidacloprid and acetamiprid) in pericarpium citri reticulatea by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Seven neonicotinoid insecticides in pericarpium citri reticulatae were extracted by acetonitrile and cleaned up by primary secondary amine (PSA), respectively. The samples were separated by chromatographic column Shim-pack XR-ODS (100 mm×2.0 mm, 3 μm), and determinated by HPLC-MS/MS with external standard method. Results The limits of detection for all pesticides were between 0.1?2 μg/kg. The calibration curves had good linear relationship in range of 0.5?50 μg/L with the correlation coefficients more than 0.9995. The recoveries were 71.0%?117.0% at 3 spiked levels with relative standard deviations of 1.8%?11.2%. Conclusion This method is simple, accurate, and well reproducible, which can meet requirements of pesticide residues detection.