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柱前衍生-高效液相色谱法测定丙戊酸钠血药浓度 被引量:16

Rapid determination of sodium valprate in serum by HPLC after precolumn derivatization
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摘要 目的 :建立快速柱前衍生 高效液相色谱法测定丙戊酸钠 (VPA)血药浓度的方法。方法 :选择 2 溴 对硝基苯乙酮为衍生试剂 ,环己烷羧酸为内标 ,Nova pakC18柱 (15 0mm× 3 9mm ,4 μm)为分析柱 ;流动相为甲醇 水 (77∶2 3,V/V) ,检测波长为 2 6 2nm ,流速 1mL·min-1,柱温 2 5℃。结果 :内标环己烷羧酸和VPA的保留时间分别为 3 0min和 4 5min ,线性范围为 2 0~ 180mg·L-1,平均回收率为 10 0 2 % ,日内、日间RSD均 <3 5 % ;2 30例服用VPA的癫患者应用本法监测 ,有 77 8%的患者血药浓度在有效浓度范围之内 ,还有 2 2 2 %的患者血药浓度低于或高于有效浓度。结论 :本法快速、简便、准确 。 AIM: To establish a rapid analysis method for the determination of sodium valprate in serum by HPLC after precolumn derivatization. METHODS: 2-Bromo-4'-nitroacetophenone was selected as derivative reagent. Cyclohexanecarboxylic acid was used as an internal standard. The analytical column was Nova-pak C 18 column (150 mm×3.9 mm,4 μm). The mobile phase consisted of methanol-water (77∶23,V/V). The detection wavelength was 262 nm and the flow rate was 1 mL·min -1,column temperature was 25℃. RESULTS: The retention time of cyclohexanecarboxylic acid and sodium valprate was 3.0 and 4.5 min,respectively. The linear range of sodium valprate was 20-180 mg·L -1. The mean relative recovery was 100.2%. The relative standard deviation (RSD) of within day and between day were all less than 3.5%. The method was used for monitoring serum sodium valprate concentration of 230 epileptic patients, 77.8% of the patients who had taken sodium valprate was found the serum concentration in effective level and 22.2% lower or higher than effective level. CONCLUSIONS: This method is found to be rapid, accurate, sensitive and more suitable for clinical practical application.
出处 《中国临床药学杂志》 CAS 2004年第2期93-96,共4页 Chinese Journal of Clinical Pharmacy
关键词 柱前衍生 高效液相色谱法 测定方法 丙戊酸钠 血药浓度 抗癫痫药物 precolumn derivatization HPLC sodium valprate serum drug concentration
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