高效液相色谱串联质谱法测定唾液中氨磷汀浓度  

Determination of Amifostine in Human Saliva by HPLC-MS/MS

作　　者：黎长江[1] 欧美贤[2] 王胜资[3] 黄滔敏[4] 陈念祖[4] 

机构地区：[1]复旦大学附属眼耳鼻喉科医院耳鼻喉科,上海200031 [2]上海市徐汇区中心医院中心实验室,上海200031 [3]复旦大学附属眼耳鼻喉科医院放疗科,上海200031 [4]复旦大学附属眼耳鼻喉科医院药剂科,上海200031

出　　处：《中国药学杂志》2013年第6期482-485,共4页Chinese Pharmaceutical Journal

摘　　要：目的建立高效液相色谱串联质谱(HPLC-MS/MS)直接检测唾液中氨磷汀(amifostine,AMI)的方法。方法收集6位健康成年志愿者唾液为基质,石杉碱甲(huperzine-A,HupA)为内标,采用蛋白沉淀法,用高效液相色谱串联质谱测定唾液中的氨磷汀。色谱柱为ZIC-HILIC亲水色谱分析柱(2.1 mm×100 mm,3.5μm),质谱分析采用多反应监测扫描模式(MRM),离子源为电喷雾离子源(ESI)。结果氨磷汀在唾液中检测到的线性范围为0.938～30 mg·L-1,线性关系良好,典型代表方程为:y=0.072x-0.005 26(r=0.999 1)(n=6),定量下限为0.938 mg·L-1(S/N>10)。唾液样品的低、中、高3个质控浓度(1.0、5.0和25 mg·L-1)批内、批间精密度(RSD)均小于15%,其方法回收率均大于85%。结论本实验所建立的氨磷汀检测方法直接、快捷、简便、灵敏度高及定性好,适用于唾液中氨磷汀的测定及科学研究。OBJECTIVE To establish an HPLC-MS/MS method （high performance liquid chromatography-tandem mass spectrometry） for the direct determination of amifostine in human saliva. METHODS Saliva samples were collected from six adult healthy volunteers. After protein precipitation and addition of the internal standard （IS） huperzine-A （HupA）, HPLC- MS/MS was used to analyze amifostine. The analysis was conducted using a ZIC^R-HILIC analytical column （2. 1 mm ×100mm,3.5μm）. Electrospray ionization was used with multiple reaction monitoring （MRM） mode. RESULTS The lower limit of quantification （LLOQ） of the method was0.938 rag· L^-1（S/N〉10）. The standard curve was linear in the range of 0.938-30 mg· L^-1（r=0.999 1, n=6）. The inter-day and intra-day RSDs were all less than 15% for the low, medium and high concentration quality control samples （1.0, 5.0 and 25 mg· L^-1 ）. The values of recovel7 were all more than 85%. CONCLUSION The method is direct, rapid, simple and sensitive, and suitable tbr the determination of amitbstine in saliva samples.

关 键 词：高效液相色谱质谱联用法 氨磷汀 唾液 

分 类 号：R917[医药卫生—药物分析学]