超高效液相色谱串联质谱法快速测定母乳中拉贝洛尔的含量
陈宇 郑新 陈立波[摘要] 目的 建立快速测定母乳中拉贝洛尔含量的超高效液相色谱串联质谱法(UPLC-MS/MS)。 方法 母乳样品经甲醇-乙腈混合溶液沉淀蛋白,稀释后离心取上清液进样。色谱柱为Thermo Scientific Syncronis C18(100 mm×2.1 mm,1.7 μm),初始流动相为0.2%甲酸溶液-乙腈(80∶20,V/V),流速为0.2 mL/min,梯度洗脱,AJS ESI正离子模式电离,多反应离子监测模式(MRM)检测,外标法定量。 结果 母乳中拉贝洛尔在1.042~104.2 ng/mL范围内线性良好(r = 0.9988),定量下限为1.042 ng/mL,准确度为92.0%~104.8%,批内、批间RSD均小于15%,提取回收率为82.2%~92.4%。 结论 本方法前处理简单、准确,专属性强、灵敏度高,可用于拉贝洛尔的乳药浓度监测。
[关键词] 拉贝洛尔;超高效液相色谱串联质谱法;乳药浓度;药物监测
[中图分类号] RTS218;O657.63 [文献标识码] A [文章编号] 1673-7210(2018)11(c)-0085-04
[Abstract] Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for rapid determination of labetalol in breast milk. Methods The breast milk sample was precipitated by a methanol-acetonitrile mixed solution, and after centrifugation, the supernatant was centrifuged for injection. The column was Thermo Scientific Syncronis C18 (100 mm × 2.1 mm, 1.7 μm), the initial mobile phase was 0.2% formic acid solution-acetonitrile (80∶20, V/V), the flow rate was 0.2 mL/min, utilizing a gradient elution program. The MS/MS detection was performed under AJS ESI+ in MRM mode ......
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