单步萃取-HPLC法同时测定人血清中3种抗癫痫药浓度

目的:建立以单步萃取-高效液相色谱法同时测定人血清中卡马西平、苯妥英钠、苯巴比妥浓度的方法。方法:血清样品采用二氯甲烷单步萃取后进样测定,色谱柱为Ultimate XB-C18,流动相为甲醇-水(70∶30),流速为1 mL·min-1,检测波长为240nm,柱温为25℃,内标为2-氨基-2-氯-5-硝基二苯酮。结果:卡马西平、苯妥英钠、苯巴比妥血药浓度分别在1.33～33.25 mg·L-1(r=0.999 6)、1.96～49.0 mg·L-1(r=0.999 5)、2.88～72.0 mg·L-1(r=0.998 8)范围内线性关系良好,最低检测限分别为0.06、0.13、0.14 mg·L-1,方法回收率分别为94.0%～109.1%、93.6%～98.7%、97.0%～105.2%,日内、日间RSD均<10%。结论:本法操作简便、快速、准确、经济实用,可满足临床快速监测的需要。

Simultaneous Determination of Serum Concentration of 3 Kinds of Anti-epilepsies Drugs by HPLC with Single Step Extraction

OBJECTIVE： To establish an HPLC method with single step extraction for the determination of the serum concentration of the carbamazepine （CBZ）, phenytoin （PHT）, phenobarbital （PBB）. METHODS： The serum samples were extracted once with dichloromethane. The residue was dissolved and analyzed with Ultimate XB-C18（250 mm×4.6 mm, 5 μm）, mobile phase was composed of methanol-water（70 ： 30） with a flow rate of 1 mL·min^-1. The detection wavelength was set at 240 nm, the colunm temperature was 25 ℃, and 2-amino-2-chloro-5-nitrobenzophenone was used as internal standard. RESULTS ： The linear range of carbamazepine, phenytoin and phenobarbital were 1.33-33.25 mg·L^-1（r=0.999 6）, 1.96-49.0 mg·L^-1（r=0.999 5） and 2.88-72.0 mg·L^-1（r=0.998 8）, respectively. The detection limit were 0.06 mg·L^-1, 0.13 mg·L^-1, 0.14 mg·L^-1. The intra-day precision and inter-day precision were less than 10%, the average recoveries were 94.0%-109.1%, 93.6%-98.7%, 97.0%-105.2%, respectively. CONCLUSION：The method is simple, rapid, accurate, economical and practical. It can be used for fast determination in the clinic.