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目的:建立牛黄消炎片中孔雀石绿的检测方法。方法:采用HPLC法鉴别和定量,使用Phenomenon Gemini C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.05 mol·L-1醋酸铵溶液(冰醋酸调pH 4.5)(40∶60)为流动相,流速1 mL·min-1,检测波长618 nm;采用HPLC-MS/MS法验证,以乙腈-5 mmol·L-1醋酸铵溶液(冰醋酸调pH 4.5)(40∶60)为流动相,电喷雾离子化源,正离子检测方式,对孔雀石绿的准分子离子峰m/z 329[M-Cl]+进行选择离子监测及二级全扫描质谱分析。结果:HPLC鉴别方法分离良好,检出限在0.03μg·mL-1;阳性样品的选择离子监测图及二级全扫描质谱图与孔雀石绿对照品一致;含量测定方法在0.33~7.85μg·mL-1线性关系良好,平均回收率为99.3%。结论:本方法专属性强,结果准确,可用于牛黄消炎片中孔雀石绿的定性、定量检测。
Objective: To establish a method for the determination of malachite green in Bezoar anti-inflammatory tablets. Methods: The HPLC method was used to identify and quantify Phenomenon Gemini C18 column (250 mm × 4.6 mm, 5 μm) with acetonitrile-0.05 mol·L-1 ammonium acetate solution (adjusted to pH 4.5 with glacial acetic acid) (40:60) The mobile phase consisted of 1 mL · min-1 of flow rate and the detection wavelength of 618 nm. The HPLC-MS / MS method was used to determine the concentration of acetonitrile in the solution of 5 mmol·L-1 ammonium acetate (40:60 with glacial acetic acid) Mobile phase, electrospray ionization source and positive ion detection method were used to monitor the quasi- ion ion peak m / z 329 [M-Cl] + of malachite green by selective ion monitoring and secondary full scan mass spectrometry. Results: The HPLC method was well separated and the detection limit was 0.03μg · mL-1. The selected ion monitoring and secondary full scan mass spectra of the positive samples were consistent with the malachite green reference substance. The content was between 0.33 ~ 7.85μg · mL-1, the average recovery was 99.3%. Conclusion: The method is specific and accurate, and can be used for the qualitative and quantitative detection of malachite green in Bezoar anti-inflammatory tablets.