气-质联用法测定血浆中阿斯匹林和水杨酸浓度及人体药代动力学研究

DETERMINATION OF ASPIRIN AND SALICYLIC ACID IN PLASMA BY GC-MS AND PHARMACOKINETIC STUDIES

目的:建立人血浆中阿斯匹林和水杨酸气相色谱质谱联用测定法,并研究了肠溶阿斯匹林片在健康人体内的药代动力学。方法:色谱柱HP525m×02mmID石英弹性毛细管柱。内标苯甲酸,血样酸化后经乙醚—二氯甲烷(4∶1)提取,BSTFA衍生化进样,采用选择离子方式检测、定量。结果:阿斯匹林、水杨酸的日内及日间的RSD分别小于478%及616%。平均回收率大于969%。最小检测浓度:阿斯匹林10ng·mL-1,水杨酸01μg·mL-1。8名健康志愿者口服单剂量50mg肠溶阿斯匹林片后,以本法测定阿斯匹林、水杨酸体内过程符合一室模型。结论:本法用于同时测定阿斯匹林和水杨酸体内浓度,灵敏度高,数据准确可靠。

AIM: To develop a GC MS method for the study of pharmacokinetics of aspirin and salicylic acid in healthy human volunteers. METHODS: A 25 m×0 2 mm ID capillary column was used. The carrier gas was helium. Benzene carbonic acid was used as internal standard. The plasma was extracted with ether—dichloromethane (4∶1) after adding 3 mol·L -1 HCl and then reacted with bis (trimethylsilyl) trifluoroacetamide (BSTFA). The concentrations of aspirin and salicylic acid were measured by GC MS (SIM). The pharmacokinetic parameters were computed using 3P87 program. RESULTS: A good linearity was obtained from 2 0～400 ng·mL -1 of aspirin and 0 2～10 0 μg·mL -1 of salicylic acid in human plasma. The detection limit of aspirin and salicylic acid were 1 0 ng·mL -1 and 0 1 μg·mL -1 in plasma, respectively. The results showed that the plasma concentration time courses conformed to one compartment model following a single oral dose of 50 mg aspirin tablets given to each of the 8 volunteers. CONCLUSION: The established GC MS method was a good method for determination of aspirin and salicylic acid in human plasma. The method was simple, precise and sensitive.