超高效液相色谱-串联质谱法测定芦蒿中7种氨基甲酸酯类农药及其代谢物残留量

UHPLC-MS/MS Determination of 7 Carbamate Pesticides and Metabolites Residues in Artemisia Selengensis

采用超高效液相色谱串联质谱法(UHPLC-MS/MS)测定芦蒿中7种氨基甲酸酯类农药及其代谢物残留。取芦蒿样品5.00g,用乙腈10mL超声提取5min,提取液用6.0g硫酸镁和1.5g乙酸钠脱水后,经QuECHERS固相萃取柱净化。净化液用(A)10mmol·L^(-1)甲酸铵溶液和(B)10mmol·L^(-1)甲酸铵-甲醇溶液的体积比为9∶1的混合液稀释至0.8mL后进行色谱分离,以Kinetex C18100A色谱柱为固定相,以不同体积比的上述两种溶液(A和B)的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正离子源和多反应监测模式。7种化合物的线性范围均在0.50~20.0μg·L^(-1)之间;检出限(3S/N)为0.17~0.55μg·kg-1。加标回收率为67.4%~103%;测定值的相对标准偏差(n=6)在1.1%~8.5%之间。

UHPLC-MS/MS was applied to the determination of 7 kinds of carbamate pesticides and metabolites residues in artemisia selengensis. Sample of artemisia selengensis （5.00 g） was extracted ultrasonically with 10 mL of acetonitrile, and the extract was dehydrated by adding 6. 0 g of MgSO4 and 1.5 g of NaOAc. The extract was then purified by passing through QuECHERS SPE columr The purified extract was diluted to 0. 8 mL with a mixture of （A） 10 mmol · L-1 ammonium formate solution and （B） 10 mmol · L-1 ammonium formate methanol solution mixed in the ratio of 9 ： 1, and the diluted solution was then separated by UHPLC using Kinetex C18 100A column as stationary phase and mixtures of ammonium formate solution of （A） and （B） mentioned above in various ratios as mobile phase in gradient elution. In MS/MS, ESI＋ and MRM were adopted. Linearity ranges for the 7 compounds were obtained to be same between 0. 50--20. 0 μg·kg-1, and values of detection limits （3S/N） found were in the range of 0. 17--0. 55 μg·kg-1. Recovery was tested by standard addition method, giving results of recovery in the range of 67. 4%--103%, and of RSDs （n=6） ranged from 1.1% to 8. 5%.