摘要
目的：建立测定人血浆中白消安浓度的高效液相色谱法。方法：血浆样品经衍生化处理后，以甲醇-水（74：26）为流动相，流速0．9mL·min^-1，选用Nova Pak C18色谱柱（3．9mm×150mm，4μm），在280nm波长下进行检测。结果：白消安血浆质量浓度的线性范围为0．050～3．20mg·L^-1，以加权最小二乘法运算得到回归方程为Y=4．575X-37．04（r=0．9993，n=9），方法回收率（100．6±1．6）%（99．66％～102．4％），血浆萃取回收率（83．6±2．4）％（81．70％～86．35％），日内和日间RSD均小于15％。检测限为0．6ng，最低血浆检测质量浓度为0．030mg·L^-1。结论：该方法准确、灵敏，适用于白消安血浆浓度测定及其药动学研究。
ORJECTIVE To develop an HPLC assay for determination of busulfan concentration in human plasma. METHODS Plasma samples were prepared by derivatization with sodium diethyldithiocarbamate（DDTC） and extracted with ethyl acetate,the extract was dried under nitrogen and reconstituted with methanol prior to HPLC determination. Chromatography was accomplished using a NovaPak C18 analytical colum （4μm,3. 9 mm× 150 mm） and mobile phase of methanol-water（74：26） at a flow rate of 0. 9 mL·min^-1 with UV detection at 280 nm. RESULTS Calibration curves were linear from 0. 05 to 3. 20 mg·L^-1 （r = 0. 999 3, n = 9）, the recovery of method was （ 100. 6 ± 1.6） % （99. 66% - 102. 4% ）, and the mean extraction yield for busulfan in plasma was （83.6 ± 2. 4） % （81.70% - 86. 35%）. The RSDs of intra- and inter-day were lower than 11.20% and 14. 99%, respectively. The limit of detection was 0. 030 mg·L^-1 （signal-to noise ratio of 6）. CONCLUSION The method is sensitive and accurate for the determination of busulfan concentration in human plasma. It is suitable for the pharmacokinetics study of busulfan.
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2007年第4期458-461,共4页
Chinese Journal of Hospital Pharmacy
基金
2007年安徽高校省级自然科学研究项目(编号KJ2007B317ZC)
