论文部分内容阅读
目的:建立柱前衍生RP-HPLC法测定人血浆中丙戊酸钠血药浓度并对监测结果进行分析。方法:环己烷羧酸为内标,2-溴-对硝基苯乙酮为衍生化试剂,Hypersil BDS C18柱(4.6 mm×200 mm,5μm)为分析柱;甲醇-水(79∶21)为流动相,检测波长为265 nm,流速1.0 mL/min,柱温30℃,用柱前衍生RP-HPLC法对10 066例次癫痫患儿进行丙戊酸钠血药浓度测定。结果:内标环己烷羧酸和丙戊酸钠衍生物的保留时间分别为6.2 min、8.1 min,丙戊酸钠浓度在13.6～326.4μg/mL范围内样品浓度与峰面积比之间线性关系良好(r=0.9989),最小可定量浓度为13.6μg/mL,平均方法回收率为95.0%～105.0%,日内日间RSD均<10%。10 066例次癫痫患儿血药浓度监测结果在治疗浓度(50～100μg/mL)内的共5 100例次,占50.7%;低于治疗浓度范围下限(<50μg/mL)共4 313例次,占42.8%;高于治疗浓度范围上限(>100μg/mL)的共653例次,占6.5%。结论:本测定方法简便快捷,灵敏准确,可用于临床丙戊酸钠血药浓度的监测;癫痫患儿应用丙戊酸钠个体差异较大,应监测其血药浓度,实施个体化给药。
OBJECTIVE: To establish a pre-column derivatization RP-HPLC method for the determination of plasma concentration of valproate in human plasma and analyze the monitoring results. METHODS: Cyclohexanecarboxylic acid was used as internal standard and 2-bromo-p-nitroacetophenone as derivatization reagent. Hypersil BDS C18 column (4.6 mm × 200 mm, 5 μm) ) As the mobile phase, the detection wavelength was 265 nm, the flow rate was 1.0 mL / min and the column temperature was 30 ℃. The plasma concentration of sodium valproate in 10 066 children with epilepsy was determined by precolumn derivatization RP-HPLC. Results: The retention times of internal standard cyclohexanecarboxylic acid and sodium valproate were 6.2 min and 8.1 min, respectively. The linearity of sample concentration to peak area ratio in the range of 13.6 ~ 326.4 μg / mL for sodium valproate The correlation was good (r = 0.9989), the minimum quantifiable concentration was 13.6μg / mL, the average recovery was 95.0% -105.0%, and the intraday RSD was less than 10%. A total of 5 100 cases (50.7%) of 10 066 children with epileptic sepsis at the therapeutic concentration (50-100 μg / mL) and 4 313 cases (lower than the lower limit of the therapeutic concentration range <50 μg / mL) Times, accounting for 42.8%; a total of 653 cases were higher than the upper limit of therapeutic concentration (> 100μg / mL), accounting for 6.5%. Conclusion: The method is simple, sensitive and accurate, and it can be used to monitor the plasma concentration of sodium valproate in children. In epilepsy patients, sodium valproate is different from each other. Mononuclear drug concentration should be monitored and monitored.