HPLC-MS/MS测定人血清中丙戊酸钠和万古霉素的浓度
投稿时间:2021-08-18  修订日期:2022-04-18  点此下载全文
引用本文:段晶晶,纪国文,郭芷君,徐峰.HPLC-MS/MS测定人血清中丙戊酸钠和万古霉素的浓度[J].药学实践杂志,2022,40(4):350~353,378
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作者单位E-mail
段晶晶 上海市奉贤区中心医院药剂科, 上海 201499  
纪国文 上海市奉贤区中心医院呼吸内科, 上海 201499  
郭芷君 上海市奉贤区中心医院药剂科, 上海 201499  
徐峰 上海市奉贤区中心医院药剂科, 上海 201499 andrewfxu@sina.com 
基金项目:上海市奉贤区科委项目(20201616);上海市卫健委青年项目(20164Y0247)
中文摘要:目的 建立同时测定人血清中丙戊酸钠和万古霉素浓度的高效液相色谱串联质谱法(HPLC-MS/MS)。方法 以丙戊酸-d6和卡那霉素B分别作为丙戊酸钠和万古霉素的内标,用乙腈沉淀蛋白法处理血清样品,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,流速为0.5 ml/min,柱温25 ℃,进样量4 μl,总分析时间12 min。采用电喷雾离子源进行正负离子模式监测,多反应监测模式进行定量分析。考察该方法的专属性、标准曲线、定量下限、精密度、回收率、基质效应以及稳定性。结果 丙戊酸钠和万古霉素分别在1~200 μg/ml和0.5~100 μg/ml范围内具有良好的线性关系,定量下限分别为1 μg/ml和0.5 μg/ml,提取回收率均达到70%以上,批间、批内精密度RSD值均小于10%,稳定性良好,无明显基质效应。结论 该方法操作简便、快捷、专属性好、灵敏度高、结果准确,可用于临床对两者同时进行血药浓度监测。
中文关键词:丙戊酸钠  万古霉素  血药浓度监测  高效液相色谱串联质谱法
 
Determination of sodium valproate and vancomycin in human serum by HPLC-MS/MS
Abstract:Objective To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of sodium valproate and vancomycin in human serum. Methods Valproic acid-d6 and kanamycin B were used as the internal standard of sodium valproate and vancomycin, the serum samples were treated by acetonitrile precipitation protein method. The mobile phase was 0.1% formic acid aqueous solution-acetonitrile for gradient elution. The flow rate was 0.5 ml/min, with column temperature at 25 ℃. The sample volume was 4 μl and total analysis time was 12 min. The positive and negative ion mode was monitored by electrospray ion source and the multiple reaction monitoring mode was used for quantitative analysis. The specificity, standard curve, lower limit of quantification, precision, recovery, matrix effect, and stability of the method were examined. Results Sodium valproate and vancomycin had good linear relationships in the range of 1 - 200 μg/ml and 0.5 - 100 μg/ml, respectively. The quantitative lower limits were 1 μg/ml and 0.5 μg/ml, respectively. The extraction recoveries were above 70%. The inter- and intra-batch precision RSD values were less than 10%. The stability was good and there was no obvious matrix effect. Conclusion This method is simple, quick, sensitive, specific and accurate, which could be used to simultaneously determine the concentration of sodium valproate and vancomycin in human serum.
keywords:sodium valproate  vancomycin  blood concentration monitoring  HPLC-MS/MS
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