| UPLC-MS/MS法测定人血浆中丙硫氧嘧啶的含量 |
| 投稿时间：2020-01-15 修订日期：2020-05-08 点此下载全文 |
| 引用本文：李群英,凌琳,李盛建,周瑾,李甜甜,赵亮,吕磊.UPLC-MS/MS法测定人血浆中丙硫氧嘧啶的含量[J].药学实践杂志,2020,38(4):350~353,378 |
| 摘要点击次数: 1322 |
| 全文下载次数: 1118 |
|
|
| 中文摘要:目的 建立UPLC-MS/MS法测定人血浆中丙硫氧嘧啶的含量，为临床治疗药物监测（TDM）和生物等效性试验（BE）提供方法学基础。方法 采用Agilent SB-C18柱（4.6 mm×150 mm，5 μm），流动相为甲醇-0.1%甲酸水溶液（80∶20，V/V），等度洗脱。质谱采用AJS-ESI源，多反应监测（MRM）正离子模式，检测离子对为：丙硫氧嘧啶m/z 171.1→112.1、内标（丙硫氧嘧啶-D5）m/z 176.1→117.0。结果 血浆中丙硫氧嘧啶在10~5 000 ng/ml范围内线性关系良好，r=0.999 3；批内和批间的精密度和准确度良好（RSD<10%，RE<±10%）；不同浓度的基质效应均<110%，变异系数<5%；不同浓度的平均回收率为101.60%~113.56%，符合方法学要求。结论 该方法快速简便、灵敏准确，适用于血浆中丙硫氧嘧啶的含量测定。 |
| 中文关键词:超高效液相色谱-串联质谱 丙硫氧嘧啶 血浆 含量测定 |
| |
| Determination of propylthiouracil in human plasma by UPLC-MS/MS |
|
|
| Abstract:Objective To establish a method for the determination of propylthiouracil in human plasma by UPLC-MS/MS and provide methodological basis for therapeutic drug monitoring (TDM) and bioequivalence test (BE) in clinical.Methods The chromatographic separation was performed on an Agilent SB-C18 column (4.6 mm×150 mm, 5 μm), the mobile phase was methanol and water containing 0.1% formic acid (80∶20, V/V), isocratic elution. MS condition was optimized in the positive ion detection mode by multiple reaction monitoring (MRM), along with the Agilent JetStream electrospray source interface (AJS-ESI). The precursors to the product ion transitions were m/z 171.1→112.1 for propylthiouracil and m/z 176.1→117.0 for the internal standard (IS).Results The calibration curve was linear in the range of 10−5 000 ng/ml for propylthiouracil in human plasma, r=0.999 3. The intra-day and inter-day precision and accuracy were good (RSD<10%，RE<±10%). The matrix effect of different concentrations was less than 110% and the coefficient of variation was less than 5%. The average recovery of different concentrations was 101.60%−113.56%, which conformed with the requirement of methodological validation.Conclusion The method is rapid, sensitive and accurate, which can be used for the determination of propylthiouracil in human plasma. |
| keywords:UPLC-MS/MS propylthiouracil plasma content determination |
| 查看全文 查看/发表评论 下载PDF阅读器 |
|
| 关闭 |
|
|
|
