摘要
目的 :建立一种简便的维拉帕米 ( Ver)及去甲基维拉帕米 ( Norv)血药浓度 HPL C- FL U的测定方法。方法 :色谱柱为Alltima C1 8柱 ( 15 0 mm× 4.6 m m,5 ︼m) ;流动相为甲醇 -水 -三乙胺 ( 5 2∶ 47.6∶ 0 .4) ,用冰醋酸调节 p H至 5 .41,流速 1ml/min。荧光检测激发波长 Ex=2 84nm,发射波长 Em=313nm。Ver和去 Norv的保留时间分别为 7.14min和 5 .17min,血样预处理采用乙腈直接沉淀法。结果 :Ver及 Norv血药浓度在 2 5～ 40 0 ng/ ml范围内线性关系良好 ( r≥ 0 .9997) ,最低检测限分别为 2 0 0 pg和 10 0 pg( r S/N≥ 3) ,最低检测浓度均为 2 0 ng/ ml。批内、批间精密度小于 5 %。结论 :本方法简便可靠 。
AIM: To develop a simple high performance liquid chromatography method for the meas urement of verapamil (Ver) and norverapamil (Norv) in serum. METHODS: Separation was obtained using a Alltima C 18 (150 mm×4 6 mm, 5 μm). The mobile phase consisted of a mixture of methanol water triethylamine (52∶47 6∶0 4) buffered to apparent pH 5 41 with acetic acid. The flow rate of mobile phase was 1 ml/min,and the rention time of Ver and Norv was 7 14 min and 5 17 min respectively. The detection was performed at 284 nm (Ex) and 313 nm (Em). The sample was precipitated by adding acetonitrile. RESULTS: Ver and Norv were linear from 25 to 400 ng·ml -1 (r≥ 0 999 7 ). The lowest detectable limit was 200 pg and 100 pg ( r S/N ≥3) respectively, and the lowest concentration was 20 ng/ml. Within day and between day coefficients of variation were less than 5%. CONCLUSION: This method is simple and reliable, and has been demonstrated to be suitable for therapeutic drug monitoring.
出处
《中国临床药学杂志》
CAS
2001年第2期99-101,共3页
Chinese Journal of Clinical Pharmacy
