LC-MS/MS方法测定人血浆中多西环素浓度

目的建立迅速、简单、灵敏的液相色谱-串联质谱法测定人血浆中多西环素的浓度。方法血浆样品采用固相萃取的方法,以含0.04%TFA的混合溶液(甲醇-乙腈-水=45∶45∶10,v/v/v)为流动相;采用Dikma C18柱(30 mm×4.6 mm,5μm)分离,通过电喷雾电离源(ESI),以选择性反应监测(SRM)方式进行正离子检测,用于定量分析的离子反应分别为m/z 444.7→428.1(多西环素)和m/z 464.6→448.0(内标,去甲金霉素)。结果建立的人血浆内多西环素测定方法线性范围为50⁵ 000 ng·mL-1,定量下限可达50 ng·mL-1。日内、日间精密度(RSD)均<12%。结论该方法预处理简洁,灵敏,专属性强,可方便用于人血浆中多西环素的测定。

LC-MS /MS determination of doxycycline in human plasma

Objective To use tandem mass spectrometric method（LC-MS/MS） to analyze doxycycline in human plasma. Methods Doxycycline and the internal standard demeclocycline were separated from the plasma by a simple solid phase extraction. Chromatographic separation was performed on a Dikma C18（30 mm×4. 6 mm, 5 μm） column with mobile phase consisting of 0.04% TFA mixed solution（methanol-acetonitrile-water = 45 ∶ 45 ∶ 10, v/v/v）. A tandem mass spectrometer equipped with electrospray ionization source was adopted as the detector. Selective reaction monitoring（SRM） transitions of m/z 444.7→428.1 and m/z 464.6→448.0 were measured in a negative mode for doxycycline and internal standard, respectively. Results The linear concentration range of the calibration curve for doxycycline was 50- 5 000 ng·mL- 1. The lower limit of quantification was 50 ng·mL- 1. The intra-day and inter-day relative standard deviation over the entire concentration range was less than 12%. Conclusion The method is sensitive and suitable for pharmacokinetic study of doxycycline in human plasma.