摘要
首次建立了牛奶中64种中性和酸性药物的高效液相色谱-串联质谱（HPLC-MS/MS）同时测定方法。样品中的残留药物用乙腈提取,经正己烷液-液分配除脂和HLB固相萃取柱净化后,以乙腈和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用HPLC-MS/MS电喷雾正离子（ESI＋）电离,多反应监测（MRM）模式检测,基质匹配外标法定量。方法的定量下限（LOQ）为1~100μg/kg,加标回收率为54%~100%,相对标准偏差小于12%。该方法操作简便,灵敏度、准确度、精密度均满足残留分析的要求。
A high performance liquid chromatography with tandem mass spectrometric（HPLC-MS/MS） method was firstly established for the simultaneous determination of multi-residue of 64 neutral and acidic drugs in milk.The samples were extracted with acetonitrile.The extracts were defatted with n-hexane by liquid-liquid partition,and purified by HLB solid-phase extraction cartridge.Acetonitrile and formic acid-ammonium acetate buffer were used as mobile phase by gradient elution.The analysis of target compounds was carried out by HPLC-MS/MS under positive electro-spray ionization（ESI＋） and multiple reaction monitoring（MRM） mode.A matrix matched external standard was used for quantitative analysis.The limits of quantification（LOQ） of the method were between 1 μg/kg and 100 μg/kg.The spiked recoveries were between 54% and 100% with RSDs less than 12%.The proposed method was simple and convenient,and its sensitivity,accuracy and precision could meet the requirements of residue analysis.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第7期645-651,共7页
Journal of Instrumental Analysis
基金
国家质检总局科技项目(2009IK314)
上海市科委技术标准专项资助项目(08DZ0505200-2)
中国检科院科研项目(2008JK002)
关键词
高效液相色谱-串联质谱
中性和酸性药物
牛奶
残留
high performance liquid chromatography with tandem mass spectrometry
neutral and acidic drugs
milk
residue
