摘要
目的建立测定人血浆中比阿培南浓度的反相高效液相色谱法。方法采用YMC-C18(150 mm×4.6 mm,5μm)柱,以0.1 mol/L醋酸钠(醋酸调pH4.5)∶乙腈=98∶2(V∶V)为流动相,流速1.0 mL/min,柱温35℃,紫外检测波长为300 nm,直接沉淀蛋白后用二氯甲烷反洗,进样0.03 mL。结果比阿培南血浆标准曲线线性范围为0.0625 mg/L^80 mg/L,最低定量限为0.0625 mg/L,预处理回收率为96.11%~98.76%,方法回收率为99.14%~109.69%,批内RSD为0.92%~2.79%,批间RSD为2.46%~4.08%。血浆样品室温放置5 h、反复冻融3次、-30℃长期保存28 d、预处理后样品进样室中放置24 h、重复进样2次,测定结果稳定,与0时刻比较变化率均小于7%。结论该方法操作简单,结果准确,重现性好,可用于人血浆中比阿培南浓度测定和药动学研究。
Objective To establish a method to determine biapenem in human plasma with high performance liquid chromatography.Methods Chromatographic separation was performed on a YMC-C18 column（150 mm×4.6 mm,5μm） eluted with a mobile phase comprising 98∶2（V∶V） of sodium acetate（0.1 mol/L,adjust with acetic acid to pH4.5） and acetonitrile with a flow rate of 1.0 mL/min.The detection wavelength was set at 300 nm.Temperature was controlled at 35 ℃.The plasma samples were precipitated with acetonitrile.The supernatant was vortexed with dichloromethane and 0.03 mL of the aqueous layer was injected for analysis.Results The method was valid to detect biapenem in a range of 0.0625 mg/L to 80 mg/L（correlation coefficient 0.999）.The pretreatment recovery of biapenem ranged from 96.11% to 98.76%.The methodological recovery of biapenem ranged from 99.14% to 109.69%.The inter-day RSD ranged from 0.92% to 2.79%.The intra-day RSD ranged from 2.46% to 4.08%.Less than 7% change of results was observed after the sample was stored in room temperature for 5 h,frozen and defrozen 3 times,stored at-30 ℃ for 28 d,stayed in autosampler for 24 h,and injected twice.Conclusion The method is sensitive,accurate and easy to perform,which offers a satisfactory tool for the determination and pharmacokinetic study of biapenem.
出处
《四川大学学报（医学版）》
CAS
CSCD
北大核心
2011年第4期564-566,共3页
Journal of Sichuan University(Medical Sciences)
