建立了小龙虾中去甲万古霉素、杆菌肽的高效液相色谱-串联质谱测定方法.样品经0.04 g/mL三氯乙酸乙腈沉淀蛋白,0.1％(v/v)酸化甲醇水溶液(4:6,V/V)提取,正己烷去脂,经C18(100 mm×2.1 mm,粒径1.9μm)柱分离,0.1％(v/v)甲酸水溶液-0.1％(v/v)甲酸乙腈溶液为流动相梯度洗脱,用电喷雾离子源正离子模式采集,多反应监测模式下检测,外标法定量.结果表明,去甲万古霉素在50～1000μg/L,杆菌肽在10～1000μg/L范围内呈良好线性关系,相关系数(r2)均>0.995,方法检出限分别为3.0μg/kg和0.6μg/kg,定量下限分别为10μg/kg和2.0μg/kg,在低、中、高3个水平添加下,去甲万古霉素的平均回收率为80.8％～96.7％,杆菌肽的平均回收率为99.5％～114％,RSD分别为2.2％～4.3％和1.1％～6.9％.该方法简便、快速,重现性好,可用于小龙虾中去甲万古霉素、杆菌肽的快速筛查.

A method for the determination of pesticides in vegetables by high performance liquid chromatography-heated electrospray ionization tandem mass spectrometry was developed.After extracted by acetonitrile and cleaned up by solid phase extraction,the samples were detected in SRM mode and quantified.The results indicated that the developed method is easier,faster and more sensitive.The linear range,recovery,precision and limits of detection can meet the requirement of residue analysis.