高效液相色谱-串联质谱法检测茶青中124种农药残留

Determination of 124 pesticide residues in tea green by high performance liquid chromatography-mass spectrometry

中文关键词:  茶青  液相色谱-串联质谱法  农药残留

英文关键词:tea green  high performance liquid chromatography-mass spectrometry  pesticide residues

中文摘要:

      目的 建立一种灵敏度高、准确性好、分析速度快, 可测定茶青中124种农药成分的高效液相色谱-串联质谱(high performance liquid chromatography-mass spectrometry, HPLC-MS)检测分析方法。方法 10 g茶青鲜叶粉末经20 mL 1%醋酸乙腈溶液提取后加入NaCl, 过氨基柱固相萃取净化。采用0.1%甲酸乙酸氨水(A), 0.1 %乙酸胺甲醇(B)作为流动相进行梯度洗脱, 选择性离子多反应监测模式扫描(selective reaction monitoring, SRM), 检测器的数据采集为分段时间窗口采集。结果 本方法在10 min内完成124种目标化合物的分离分析。124种目标化合物的0.05、0.2 mg/kg添加水平的回收率为75.3%~93.6%, 相对标准偏差小于8.5%(n=6), 方法定量限为0.3 mg/kg。结论 该方法快速、准确、灵敏, 适合测定茶青中124种药物残留。

英文摘要:

      Objective To establish a method for the determination of 124 pesticides in tea green with high sensitivity, good accuracy and fast analysis speed by high performance liquid chromatography-mass spectrometry (HPLC-MS). Methods The 10 g fresh tea leaf powder was extracted by 20 mL 1% acetonitrile acetate solution, then added NaCl and purified by solid phase extraction with amino column. Gradient elution was carried out using 0.1% formic acid ammonia acetate (A) and 0.1% acetamidomethanol (B) as mobile phases, and selective reaction monitoring mode (SRM) was used. The data of the detector was collected by time windows. Results This method could complete the separation and analysis of 124 target compounds within 10 min. The recoveries at 2 spiked levels (0.05 and 0.2 mg/kg) of 124 target compounds were ranged from 75.3% to 93.6%, with the relative standard deviations (RSDs) less than 8.5% (n=6), and the limits of quantitation (LOQ) for the 124 pesticides were 0.3 mg/kg Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting 124 pesticides in tea green.