摘要
建立了用ＨＰＬＣ同时测定人血清中硫唑嘌呤（ＡＺＰ）和６－巯基嘌呤（６－ＭＰ）浓度的方法。血清样品经乙腈除蛋白后在常压和３７℃下用氮气吹干，残余物用１００μＬ洗脱液溶解，离心后上清液直接进样。以ＳｐｈｅｒｉｓｏｒｂＣ１８固定相，采用梯度洗脱，从Ｖ（乙腈）∶Ｖ（０．０１ｍｏｌ／Ｌ磷酸二氢钾）＝３∶９７经５ｍｉｎ时变为１８∶８２，１５ｍｉｎ后再变为５０∶５０，检测波长开始为３２５ｎｍ，１０ｍｉｎ后为２７８ｎｍ，甲硝唑（ＭＮＺ）为内标。ＡＺＰ和６－ＭＰ平均回收率分别为（１００．６±４．２）％和（１０２．４±４．５）％，最低检出质量浓度均为５μｇ／Ｌ。所建方法简便、灵敏、准确。
A method for simultaneous determination of azathiopurine(AZP) and its metabolite 6 mercaptopurine(6 MP) concentration in serum has been developed. Rreversed phase high performance liquid chromatography with gradient elution and dualwavelength detection was employed. After protein precipitation with acetonitrile, the serum sample was evaporated to dryness with a gentle N 2 stream at 37℃ and 100 μL of the mobile phase were added to dissolve the residue. After centrifugation, 20 μL of the supernatant was injected diretly into the HPLC. The detection wavelength was set at 278 nm (AZP) and 325 nm (6 MP). The internal standard was metronidazole. The minimum detectable mass concentration for both AZP and 6 MP in serum was 5 mg/L. The average recoveries were (100.6±4.2)% for AZP and (102.4±4.5)% for 6 MP.
出处
《色谱》
CAS
CSCD
北大核心
1998年第6期513-515,共3页
Chinese Journal of Chromatography
关键词
硫唑嘌呤
巯嘌呤
血药浓度
HPLC
免疫抑制剂
high performance liquid chromatography, azathiopurine, serum drug concentration
