论文部分内容阅读
目的:建立测定胎盘灌流液中格列本脲浓度的超快速液相色谱-串联质谱(UFLC-MS/MS)方法。方法:以格列齐特为内标,胎盘灌流液样品用乙腈沉淀蛋白后进样分析。采用Shim-pack XR-ODS II C18(2.0 mm×75 mm,2.2μm)色谱柱,以0.1%(v/v)甲酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱(0~0.5 min,90%A,10%B;0.5~1.5 min,90%A→10%A,10%B→90%B;1.5~2.7 min,10%A,90%B;2.7~3.5 min,90%A,10%B),流速0.4 mL·min-1。质谱采用多反应监测(MRM)扫描模式,以电喷雾离子源(ESI)在正离子电离模式下进行测定,格列本脲和格列齐特的定量分析离子分别为m/z494.0→369.0和m/z 324.1→110.1。结果:胎盘灌流液中格列本脲浓度在0.25~250 ng·mL-1范围内线性关系良好(r=0.9998),日内及日间RSD均小于15%,稳定性考察结果良好。结论:该方法快速、灵敏,专属性强,可用于胎盘灌流液中格列本脲浓度的测定。
Objective: To establish an ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS / MS) method for the determination of glibenclamide in placental perfusate. Methods: Gliclazide was used as an internal standard. Samples of placental perfusate were precipitated with acetonitrile and injected into the sample. The mobile phase was eluted with 0.1% (v / v) formic acid (A) -acetonitrile (B) using a Shim-pack XR-ODS II C18 column (2.0 mm × 75 mm, 0.5 to 1.5 min, 90% A to 10% A, 10% B to 90% B; 1.5 to 2.7 min, 10% A to 90% B; 90% A, 10% B) at a flow rate of 0.4 mL · min -1. Mass spectrometry was performed in multiple reaction monitoring (MRM) scan mode with electrospray ionization (ESI) in positive ionization mode. Quantitative analysis of glyburide and gliclazide was m / z 494.0 → 369.0 And m / z 324.1 → 110.1. Results: The linearity of glibenclamide in placental perfusate ranged from 0.25 to 250 ng · mL-1 (r = 0.9998). The intra-day and inter-day RSD were less than 15%, and the stability was good. Conclusion: The method is rapid, sensitive and specific and can be used to determine the concentration of glibenclamide in placental perfusate.