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目的建立测定人血浆中西酞普兰浓度的超高效液相串联质谱法,观察西酞普兰在血浆中的稳定性。方法流动相为体积分数0.05%甲酸溶液-乙腈(30∶70),流速为0.1mL/min,进样量为5L,柱温为35℃,样品室温度为4℃。采用Agela公司Venusil MP C18色谱柱(2.1mm×50mm,3μm)分离,通过电喷雾离子化四极杆串联质谱,以多反应监测方式进行检测。用于定量分析的离子反应分别为m/z 325.22→109.25(西酞普兰)和m/z 265.23→167.37(内标盐酸苯海拉明)。结果西酞普兰的线性范围为0.55~137.04μg/L,日内、日间精密度相对标准差均<10%;血浆中西酞普兰低、中、高浓度水平的提取回收率分别为(89.6±2.1)%、(72.4±0.6)%、(86.3±2.5)%,内标为(77.2±0.7)%,相对回收率分别为(92.6±7.0)%、(100.7±7.3)%、(106.4±4.4)%;西酞普兰血样长期冷冻稳定性、标准品溶液及内标贮备液长期稳定性、多次冻融稳定性、室温稳定性均较佳。结论本研究建立的分析方法快速、准确、灵敏、简便,适用于西酞普兰血浆药物浓度测定。
OBJECTIVE To establish a method for the determination of citalopram in human plasma by ultra performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) and observe the stability of citalopram in plasma. The mobile phase consisted of 0.05% formic acid and acetonitrile (30:70), the flow rate was 0.1 mL / min, the injection volume was 5L, the column temperature was 35 ℃, and the sample compartment temperature was 4 ℃. Separation by Agela Venusil MP C18 column (2.1 mm × 50 mm, 3 μm) was performed by electrospray ionization quadrupole tandem mass spectrometry and detected by multiple reaction monitoring. The ion reactions used for the quantitative analysis were m / z 325.22 → 109.25 (citalopram) and m / z 265.23 → 167.37 (diphenhydramine hydrochloride internal standard) respectively. Results The linear range of citalopram was 0.55 ~ 137.04 μg / L. The relative standard deviations of intracranial and intracranial precision were all less than 10%. The recoveries of low, medium and high concentrations of citalopram in plasma were 89.6 ± 2.1 ), (72.4 ± 0.6)%, (86.3 ± 2.5)% and internal standard (77.2 ± 0.7)% respectively. The relative recoveries were 92.6 ± 7.0%, 100.7 ± 7.3% and 106.4 ± 4.4, ); Citalopram long-term frozen stability of blood samples, standard solution and internal standard stock solution long-term stability, multiple freeze-thaw stability, room temperature stability are better. Conclusion The analytical method established in this study is rapid, accurate, sensitive and simple and suitable for the determination of citalopram in plasma.