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

中文关键词:  氯虫苯甲酰胺  蜂蜜  液液萃取  高效液相色谱-串联质谱法  高效液相色谱法

英文关键词:chlorantraniliprole  honey  liquid liquid extraction  high performance liquid chromatography-tandem mass spectrometry  high performance liquid chromatography

中文摘要:

      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1.25~50.00 μg/L范围内线性相关性良好, 相关系数r2为0.9996; 在1、2、5 μg/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0.5 μg/kg, 定量限为1.0 μg/kg。高效液相色谱法在25~1000 μg/L范围内线性相关性良好, 相关系数r2为0.9995; 在20.0、50.0、100.0 μg/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10 μg/kg, 定量限为20 μg/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。

英文摘要:

      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?50.00 μg/L, and the correlation coefficient r2 was 0.9996; the recoveries of standard addition at the mass concentration levels of 1, 2 and 5 μg/kg were 90.5%?105.9%, the relative standard deviations were 2.9%?4.6% (n=6); the limit of detection was 0.5 μg/kg, and the limit of quantification was 1.0 μg/kg. The high performance liquid chromatography had a good linear correlation in the range of 25?1000 μg/L, and the correlation coefficient r2 was 0.9995; the recovery rates of standard addition at the mass concentration levels of 20.0, 50.0 and 100.0 μg/kg were 94.6%?104.4%; the relative standard deviations were 1.6%?2.9% (n=6); the limit of detection was 10 μg/kg, and the limit of quantification was 20 μg/kg. Conclusion This method is accurate, sensitive and rapid, which is suitable for the determination of chlorantraniliprole residues in honey.