高效液相色谱串联质谱法测定豆芽中4种药物残留

摘要

建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)同时测定豆芽中4种药物残留的方法.豆芽经酸化乙腈匀浆提取,无水硫酸镁和十八烷基硅烷(C18)粉末分散固相萃取净化,以乙酸铵溶液和乙腈为流动相,洗脱分离后,采用多反应监测(multiple reactions monitoring,MRM)检测,基质匹配标准溶液外标法定量.结果表明,赤霉素、6-苄基腺嘌呤、4-氯苯氧乙酸、2,4-滴在1.0 μg/L~200.0 μg/L的范围内,其浓度与各待测物的峰面积呈良好的线性关系,相关系数均大于0.9997,样品添加回收试验的平均回收率为63.8 %~119.0 %,相对标准偏差为1.94 %~12.34 %之间(n=6).该方法简单准确,适用于豆芽中4种药物残留的同时检测.%A method for the simultaneous determination of four drug residues(6-benzylaminour,gibberellic acid, 4-chlorophenoxyacetic acid, 2,4-dichlorophenoxyacetic acid)in bean sprouts by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed.The samples were extracted with acetonitrile containing 5 % acetic acid,followed by clean-up using the powder of magnesium sulfate and C18. The resulting samples were separated on a C18 column, and detected by multiple reactions monitoring (MRM)under the condition of Negative mode. The results showed that the linear calibration curves were obtained in the entire range(1.0 μg/L-200.0 μg/L)for all the above rug residues,with the correlation coefficients higher than 0.999 7.For all the samples,the average spiked recoveries ranged 63.8 % from 119.0 %,and the relative standard deviations(RSDs,n=6)were in the range of 1.94 %-12.34 %. The method is easy and accurate,and can meet the requirement for the determination of four drug residues in bean sprouts.