高效液相色谱法测定抗癫痫类中成药中6种非法添加的化学药物

HPLC Determination of 6 Chemical Drugs Illicitly Added to Anti-Epilepsy Ready-Made Traditional Chinese Medicines

应用高效液相色谱法测定抗癫痫类中成药中苯巴比妥、苯妥英钠、卡马西平、氯硝西泮、丙戊酸钠和地西泮等6种非法添加的化学药物的含量。中成药样品经甲醇提取,所得提取液以Kromasil C18色谱柱为分离柱,用(A)0.01mol·L-1磷酸二氢钾溶液(用磷酸调至pH 2.5)-乙腈(90+10)混合溶液和(B)乙腈两者的不同比例的混合液作为流动相进行梯度洗脱,在检测波长210nm处进行测定。丙戊酸钠的质量浓度为200~4 000mg·L-1,其余5种化合物均在5~100mg·L-1范围内与各相应峰面积之间呈线性关系。方法的检出限(3S/N)在1~20mg·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在98.0%~103%之间,测定值的相对标准偏差(n=6)在0.41%~1.9%之间。

HPLC was applied to the determination of 6chemical drugs,i.e.phenobarbital,phenytoin,carbamazepine,clonazepam,sodium vedproate and diazepam illicitly added to anti-epilepsy ready-made traditional Chinese medicines.The TCM sample was extracted with methanol.Kromasil C18chromatographic column was used as stationary phase,and mixtures of(A)mixed solution of 0.01mol·L-1 KH2PO4(adjusted to pH 2.5with H3PO4)solution and CH3CN(90+10)and(B)acetonitrile with various proportions were used as mobile phase in the gradient elution.UV-detection at 210nm was adopted in the determination.Linear relationships were kept between values of peak area and mass concentration of sodium vedproate in the range of 200-4 000mg·L-1 and of the remainder 5drugs in the same range of 5-100mg·L-1.Detection limits(3S/N)found were ranged from 1to20mg·L-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 98.0%-103%,with RSD′s(n=6)in the range of 0.41%-1.9%.