| 用LC-MS法测定人血浆中顺式阿曲库铵的浓度 |
| 投稿时间：2019-09-01 修订日期：2020-01-09 点此下载全文 |
| 引用本文：辛博,万丽丽,王婧,刘金变,霍炎,郭澄.用LC-MS法测定人血浆中顺式阿曲库铵的浓度[J].药学实践杂志,2020,38(2):148~151 |
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| 基金项目:上海市科委科研计划项目(16DZ191110A)；上海市科委科研计划项目(16DZ1911109) |
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| 中文摘要:目的 建立高效液相色谱串联质谱方法（LC-MS）测定人血浆中顺式阿曲库铵的浓度，并应用于临床治疗药物监测。方法 采用盐酸普罗帕酮同位素内标，样品经2%甲酸水和含内标的乙腈溶液沉淀蛋白处理。HPLC色谱柱为Agilent SB-C18，柱温35 ℃，流速0.3 ml/min，流动相为0.1%甲酸水和0.1%甲酸乙腈溶液，梯度洗脱。质谱检测方式为ESI正离子模式，MRM扫描，监测阿曲库铵m/z 464.6~358.4，盐酸普罗帕酮（内标）m/z 342.2~116.2。结果 人血浆中顺式阿曲库铵在该条件下分离良好，在2~500 ng/ml浓度范围内线性关系良好（r=0.996 5），定量下限为2 ng/ml。方法日内精密度RSD<16.0%；日间精密度RSD<6.0%。平均回收率为97.63%~111.93%；血浆样品室温放置4 h，-80 ℃放置14 d，处理后室温放置24 h，稳定性良好。结论 本方法简便、准确、快速、稳定，适用于顺式阿曲库铵的血药浓度测定。 |
| 中文关键词:顺式阿曲库铵 高效液相色谱串联质谱 人血浆 治疗药物监测 |
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| Cisatracurium assay in human plasma by LC-MS |
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| Abstract:Objective To establish a LC-MS method of cisatracurium assay in human plasma for clinical therapeutic drug monitoring.Method Propafenone Hydrochloride was used as the internal standard. The plasma samples were treated with 2% formic acid aqueous solution and acetonitrile containing the internal standard to precipitate protein. Agilent SB-C18 column was used for gradient elution with the mobile phase of 0.1% formic acid-water and 0.1% formic acid-acetonitrile solution at 35 ℃ and 0.3 ml/min flow rate. The degradation products of cisatracurium m/z 464.6-358.4 and propafenone hydrochloride m/z 342.2-116.2 were identified by ESI positive-ion detection.Results There was a linear rage of cisatracurium in 2-500 ng/ml (r=0.996 5) with a detection limit of 2 ng/ml. The intra-day coefficients of variation (CVs) were less than 16.00%, and the inter-day CVs were less than 6.00%. The mean recoveries were in the range of 97.63%-111.93%. The plasma samples were stable for 4 hours at room temperature, 14 days at -80 ℃ and 24 hours after pretreated.Conclusion This method was simple, accurate, fast and repeatable for the cisatracurium assay in human plasma. |
| keywords:cisatracurium LC-MS human plasma therapeutic drug monitoring |
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