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目的建立简单超快速液相色谱—质谱/质谱联用法测定氯丙嗪制剂中氯丙嗪的含量。方法样品以乙醇提取、微孔滤膜滤过、离心后,通过电喷雾离子化(ESI),采用多反应检测方式进行正离子检测,用于定量分析的检测离子为质荷比319.0→85.8。采用Shim-pack XR-ODS(3.0 mm×75 mm,2.0μm)柱分离,以乙腈—水—甲酸(90∶10∶0.02,V/V/V)为流动相,流速为0.40 m L/min,在3 min内完成氯丙嗪定量分析。结果线性范围为1~256 ng/m L,最低检测限为1 ng/m L;日内、日间测定的相对标准偏差分别小于1.34%、1.89%。结论本方法重复性好,灵敏度高,分析速度快,操作简单,可作为氯丙嗪制剂中氯丙嗪质量控制方法。
Objective To establish a simple ultra-fast liquid chromatography-mass spectrometry / mass spectrometry method for the determination of chlorpromazine in chlorpromazine preparations. Methods The samples were extracted with ethanol, filtered through a microporous membrane filter, centrifuged, and electrospray ionized (ESI) was used to detect the positive ions by a multiplex reaction method. The mass of the detected ions for the quantitative analysis was 319.0 → 85.8. The column was separated on a Shim-pack XR-ODS (3.0 mm × 75 mm, 2.0 μm) column using acetonitrile-water-formic acid (90:10:0.02, V / V / V) as mobile phase at a flow rate of 0.40 m L / min , Within 3 min chlorpromazine quantitative analysis. Results The linear range was 1 ~ 256 ng / m L with the minimum detection limit of 1 ng / m L. The relative standard deviations (RSDs) were less than 1.34% and 1.89%, respectively. Conclusion The method has good repeatability, high sensitivity, fast analysis speed and simple operation. It can be used as a quality control method of chlorpromazine in chlorpromazine preparation.