摘要
目的:建立柱前衍生HPLC法测定人血浆中白消安浓度。方法:以1,5-戊二醇二甲磺酸酯为内标,经二乙基二硫代氨基甲酸钠(DDTC)衍生化处理后,采用HPLC-紫外法进行测定。色谱柱:NovaPak C_(18)柱(150 mm×3.9 mm,4μm),柱温:30℃,流动相:甲醇-水(74:26),流速:0.9 ml·min^(-1),检测波长:280 nm,进样量:30μl。结果:白消安血药浓度的线性范围为0.050～3.500 mg·L^(-1)(r=0.999 7),定量下限为0.050 mg·L^(-1),低、中、高3个浓度的日内RDD分别为1.65%,2.95%,6.26%,日间RSD分别为5.61%,5.71%,12.41%,提取回收率分别为82.59%,84.19%,86.70%。应用本法测定1例采用白消安静滴方案患者的血药浓度,并将结果与LC-MS/MS法测得的数据进行比较,得到直线回归方程为Y=0.945X+13.237,r=0.992 2。结论:本方法简便可靠、专一性好,适用于白消安的血浆浓度测定,能满足白消安药动学研究需求。
Objective：To develop an HPLC method for the determination of busulfan in human plasma.Method：Totally 200μl plasma sample with 1,5-pentanediol dimethyl sulfonate as the internal standard was treated by pre-column derivation with sodium diethyldithiocarbamate （DDTC）.An HPLC-UV method was adopted.A chromatographic column of NovaPak C_（18）（150 mm×3.9 mm,4μm） was used and the column temperature was 30℃.The mobile phase was composed of methanol-water（74：26） at a flow rate of 0.9 ml·min^（-1） with detection wavelength at 280 nm.The injection volume was 30μl.Result：The linear range was 0.050-3.50 mg·L^（-1） （r =0.999 7） with the determination limit of 0.050 mg·L^（-1）.The intra-day RSDs were 1.65%,2.95%and 6.26%,and the interday RSDs were 5.61%,5.71%and 12.41%,respectively.The extract recoveries were 82.59%,84.19%and 86.70%.The method was applied to determine plasma samples from one patient with intravenous injection of busulfan.The linear regression equation and correlation coefficient was as follows：Y = 0.945X ＋ 13.237 and 0.992 2,respectively by comparing the results measured by HPLC and LC-MS/MS.Conclusion：The developed method is simple,reliable and selective in the determination of busulfan in human plasma, and suitable for the pharmacokinetic study of busulfan.
出处
《中国药师》
CAS
2013年第3期395-397,共3页
China Pharmacist
