摘要
目的改进测定人血清中丙戊酸镁浓度的高效液相色谱法。方法血清样品经1.0 mol/L硫酸沉淀,以环己甲酸为内标,以2-溴-4'-硝基苯乙酮为衍生试剂。采用高效液相色谱法测定,色谱柱为Hypersil C_(18)柱(200 mm×4.6 mm,10μm),流动相为甲醇-水(81∶19),检测波长为265 nm,流速为1.0 m L/min,柱温为25℃。并对2016年度医院216份质控样本进行统计分析。结果内标和丙戊酸镁衍生物的保留时间分别为4.1 min和5.4 min,质量浓度线性范围为11.0~200.0μg/m L(r=0.999 3),平均回收率为98.2%~102.5%,批内、批间精密度RSD<2.3%,稳定性试验RSD<3.9%,2016年度质控数据批间RSD<15%,符合2015年版《中国药典(四部)》要求。2016年度质控基本符合正态分布,所有质控数据均为在控。结论改进后的方法简便、快速、准确,适用于临床丙戊酸镁血药浓度监测,室内质控评价保证了血药浓度监测质量。
Objective To improve the HPLC method for determining the concentration of magnesium valproate in human serum. Methods The serum was precipitated by sulfuric acid （ 1. 0 mol/L ） , the cyclohexane carboxylic acid was used as an internal standard and 2-bromo-4′-nitroacetophenone was used as derivation agent. The HPLC method was used, the chromatographic column was C18 column （ 200 mm × 4. 6 mm, 10 μm ） , the mobile phase was methanol-water （ 81：19 ） , the detection wavelength was 265 nm, the flow rate was 1. 0 mL/min, and the column temperature was 25 ℃. Totally 216 quality control samples of the hospital in 2016 were statisti-cally analyzed. Results The retention time of cyclohexanecarboxylic acid derivate and magnesium valproate derivative were 4. 1 min and 5. 4 min, respectively, the linear range was 11. 0-200. 0 μg/mL （ r=0. 9993 ） , and the average recovery was 98. 2% -102. 5%, the RSDs of within batch and between batch were less than 2. 3%, RSD of stability was less than 3. 9%, RSD of quality control data in 2016 were less than 15%, which accorded with the requirement of Chinese Pharmacopoeia （ 2015 Edition, Volume Ⅳ） . The quality control basically accorded with the normal distribution in 2016, and all the quality control data were in control. Conclusion The improved method is simple, rapid and accurate, it is suitable for monitoring the concentration of magnesium val-proate in serum, and the internal quality control ensures the monitoring quality of serum concentration.
出处
《中国药业》
CAS
2017年第23期10-13,共4页
China Pharmaceuticals
基金
武汉药学会医院药学研究基金[武药会201502003]
关键词
丙戊酸镁
高效液相色谱法
血药浓度监测
质控评价
magnesium valproate
HPLC
blood concentration monitoring
assesssment of quality control
