QuEChERS-超高效液相色谱-串联质谱法同时测定苦水玫瑰中6种氨基甲酸酯类及3种烟碱类杀虫剂

Determination of 6 kinds of carbamate pesticides and 3 kinds of chloronicotinyl pesticides in Chinese Kushui rose by ultra high performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS

目的建立QuEChERS-超高效液相色谱-串联质谱同时测定苦水玫瑰中6种氨基甲酸酯类及3种烟碱类杀虫剂的方法。方法苦水玫瑰样品粉碎后乙腈超声提取,经过QuEChERS分离净化后通过C_(18)色谱柱(2.1 mm×100 mm,1.7μm),以含0.1%甲酸的10 mmol/L乙酸铵-乙腈溶液进行梯度洗脱,采用电喷雾电离正离子(ESI+)多反应监测(MRM)模式检测,外标法定量。结果9种农药在0.01~0.50μg/mL浓度范围内线性相关系数(r)>0.990,加标回收率为76.3%~102%,相对标准偏差(RSD)为1.3%~9.0%(n=6),方法检出限和定量限分别为0.0016~0.0032和0.0054~0.010 mg/kg。结论本方法可以快速、简单、准确的同时检测苦水玫瑰中6种氨基甲酸酯类和3种烟碱类杀虫剂,适用于日常苦水玫瑰的检测。

Objective To establish a method for determination of 6 kinds of carbamate pesticides and 3 kinds of chloronicotinyl pesticides in Chinese Kushui rose by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)coupled with QuEChERS.Methods After extracted by acetonitrile,the Chinese Kushui rose was cleaned by QuEChERS.The target compounds were separated by C18 column(2.1 mm×100 mm,1.7μm)using 10 mmol/L ammonium acetate solution(0.1%formic acid)with acetonrtrile as mobile phase for gradient elution,and analyzed by MS/MS system with electrospray ionization(ESI+)under muti-reaction monitoring mode and quantified by external standard method.Results All the 9 kinds of pesticides showed good linear relationships in range of 0.01-0.50μg/mL,and the correlation coefficients were above 0.990,the recoveries at different spiked levels for all target compounds in blank matrices were 76.3%-102%,and the relative standard deviation(RSD)were 1.3%-9.0%(n=6).The limits of detection and quantification of the method were 0.0016-0.0032 and 0.0054-0.010 mg/kg.Conclusion The method was suitable for rapid screening and analysis of 9 pesticide residues in Chinese Kushui rose with the advantage of accuracy,rapidity,simplicity and high sensitivity.