高效液相色谱-串联质谱法和高效液相色谱法测定蜂蜜中氯虫苯甲酰胺残留量

Determination of chlorantraniliprole residues in honey by high performance liquid chromatography-tandem mass spectrometry and high performance liquid chromatography

目的建立通过一次样品前处理,可供高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)和高效液相色谱法(high performance liquid chromatography,HPLC)2种仪器检测蜂蜜中氯虫苯甲酰胺残留量的方法。方法试样经1%乙酸水溶解,乙酸乙酯萃取,氮吹浓缩,乙腈-水(1:1,V:V)复溶,供仪器检测,外标法定量。结果高效液相色谱-串联质谱法在1.25~50.00μg/L范围内线性相关性良好,相关系数r^(2)为0.9996;在1、2、5μg/kg质量浓度水平下的加标回收率为90.5%~105.9%,相对标准偏差为2.9%~4.6%(n=6);检出限为0.5μg/kg,定量限为1.0μg/kg。高效液相色谱法在25~1000μg/L范围内线性相关性良好,相关系数r2为0.9995;在20.0、50.0、100.0μg/kg质量浓度水平下的加标回收率为94.6%~104.4%,相对标准偏差为1.6%~2.9%(n=6);检出限为10μg/kg,定量限为20μg/kg。结论本方法快速、准确、灵敏,适用于蜂蜜中氯虫苯甲酰胺残留量的测定。

Objective To establish a method for the detection of chlorantraniliprole residues in honey by 2 kinds of instruments including high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)and high performance liquid chromatography(HPLC)through one sample pretreatment.Methods The samples were dissolved in 1%acetic acid water and extracted with ethyl acetate.The extract was concentrated by nitrogen blowing,redissolved with acetonitrile-water(1:1,V:V),and detected by HPLC-MS/MS and HPLC.The results were quantified by external standard method.Results High performance liquid chromatography-tandem mass spectrometry had a good linear correlation in the range of 1.25-50.00μg/L,and the correlation coefficient r^(2) was 0.9996;the recoveries of standard addition at the mass concentration levels of 1,2 and 5μg/kg were 90.5%-105.9%,the relative standard deviations were 2.9%-4.6%(n=6);the limit of detection was 0.5μg/kg,and the limit of quantification was 1.0μg/kg.The high performance liquid chromatography had a good linear correlation in the range of 25-1000μg/L,and the correlation coefficient r;was 0.9995;the recovery rates of standard addition at the mass concentration levels of 20.0,50.0 and 100.0μg/kg were 94.6%-104.4%;the relative standard deviations were 1.6%-2.9%(n=6);the limit of detection was 10μg/kg,and the limit of quantification was 20μg/kg.Conclusion This method is accurate,sensitive and rapid,which is suitable for the determination of chlorantraniliprole residues in honey.