超高效液相色谱法测定阿司匹林和水杨酸的血药浓度

An UPLC method for determination of aspirin and salicylic acid in human plasma

目的:建立并验证超高效液相色谱法(UPLC)测定人血浆中阿司匹林(ASP)和水杨酸(SA)的浓度,并应用于临床ASP和SA血药浓度的测定。方法:色谱柱为ACQUITYUPLC~BEH C_(18)(2.1 mm×100 mm,1.7μm),流动相为含0.05%三氟乙酸(TFA)的超纯水和乙腈(78%∶22%),流速0.5 mL·min^(-1),柱温30℃,进样器4℃,检测波长304 nm和277 nm,内标为替硝唑。结果:ASP和SA分别在0.4~100μg·mL^(-1)和0.2~50μg·mL^(-1)线性关系良好(r^2>0.999);ASP和SA的日内、日间准确度和精密度均<15%。结论:本研究建立了一个准确、灵敏且稳定的UPLC法测定ASP和SA血药浓度的方法,可应用于临床ASP和SA血药浓度的测定和药动学研究,指导临床合理用药。

OBJECTIVE To develop and validate an UPLC method for determination of aspirin（ASP）and salicylic acid（SA）in human plasma.METHODS Aspirin and salicylic acid were analyzed on an ACQUITY UPLC- BEH C18（2.1 mm×100 mm,1.7μm）column,with water（0.05%trifluoroacetic acid）and acetonitrile（78%∶22%）as mobile phase,flow rate at0.5 mL·min^-1.The temperatures of column and autosampler were kept at 30 ℃ and 4 ℃,respectively.The detecting wavelengths were set at 304 nm and 277 nm,and tinidazole was chosen as internal standard.RESULTS The calibration curves of ASP and SA were linear（r^2〉0.999）in the range of 0.4-100μg·mL^-1and 0.2-50μg·mL^-1,respectively.The precision and accuracy of intra-day and inter-day were all less than15%.CONCLUSION The UPLC method developed in this study for determination of ASP and SA in human plasma is accurate,sensitive and stable,and is applicable for clinical pharmacokinetic study.