| UHPLC-MS/MS测定人血浆中尿嘧啶与二氢尿嘧啶的浓度 |
| 投稿时间：2021-02-05 修订日期：2021-06-03 点此下载全文 |
| 引用本文：童萃,陈顺,王志鹏,高守红.UHPLC-MS/MS测定人血浆中尿嘧啶与二氢尿嘧啶的浓度[J].药学实践杂志,2021,39(4):348~351,365 |
| 摘要点击次数: 697 |
| 全文下载次数: 563 |
|
| 基金项目:上海市科委医学引导项目（17411972400） |
|
| 中文摘要:目的 建立同时测定人血浆中尿嘧啶(U)和二氢尿嘧啶(UH2)含量的超高效液相色谱串联质谱（UHPLC-MS/MS）方法。方法 在Agilent 6460A串联质谱仪上采用正离子检测模式，以氯尿嘧啶为内标，3%牛血清蛋白为代血浆基质，样本经乙酸乙酯液液萃取后在Agilent poroshell 120 SB-Aq (2.1 mm×100 mm，2.7 μm)色谱柱上采用梯度洗脱进行色谱分离。流动相为5 mmol/L醋酸铵水溶液和乙腈溶液；流速0.3 ml/min；柱温为30 ℃；进样量为5 μl。结果 尿嘧啶和二氢尿嘧啶的线性范围为10.0~1500.0 ng/ml，线性关系良好，其相关系数r>0.990，日内与日间精密度偏差均<15%。结论 该方法操作简单、选择性好，可用于测定人血浆中尿嘧啶和二氢尿嘧啶的含量。 |
| 中文关键词:超高效液相串联质谱法 尿嘧啶 二氢尿嘧啶 含量测定 |
| |
| UHPLC-MS/MS determination of uracil and dihydrouracil in human plasma |
|
|
| Abstract:Objective To establish an UHPLC-MS/MS method for the determination of uracil (U) and dihydrouracil (UH2) in human plasma.Methods A positive ion detection mode was adopted on the Agilent 6460A mass spectrometer. Chlorouracil was used as the internal standard. 3% bovine serum albumin was used as surrogate plasma matrix. The pretreatment of plasma sample was completed based on liquid-liquid extraction with ethyl acetate. The chromatographic separation was achieved on an Agilent Poroshell 120 SB-Aq (2.1 mm×100 mm, 2.7 μm) column with gradient elution. The mobile phase was 5 mmol/L ammonium acetate aqueous solution and acetonitrile solution. The flow rate was 0.3 ml/min. The column temperature was 30°C. The injection volume was 5 μl.Results The linear range of uracil and dihydrouracil was 10.0-1500.0 ng/ml. Both of uracil and dihydrouracil had good linear relationship with correlation coefficient (r)>0.990. Both of inter- and intra-day precision was <15%.Conclusion The established method is simple, selective, and suitable for the determination of U and UH2 in human plasma. |
| keywords:UHPLC-MS/MS uracil dihydrouracil content determination |
| 查看全文 查看/发表评论 下载PDF阅读器 |
|
| 关闭 |
