牛黄消炎片中孔雀石绿的检测方法研究  

Study on detection of malachite green in Niuhuang Xiaoyan tablets

作　　者：何风艳[1] 何轶[1] 余新启 宿威 戴忠[1] 鲁静[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]湖北省黄石市食品药品检验所,黄石435000 [3]北京市西城区药品检验所,北京100037

出　　处：《药物分析杂志》2014年第4期698-701,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：公益性行业科研专项资助项目(2012104008-1)

摘　　要：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（250mm×4．6mm，5μm），以乙腈-0．05mol·L^-1醋酸铵溶液（冰醋酸调pH4．5）（40：60）为流动相，流速1mL·min^-1，检测波长618nm；采用HPLC—MS／MS法验证，以乙腈-5mmol·L^-1醋酸铵溶液（冰醋酸调pH4．5）（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／z329[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 develop a specific method for the detection of malachite green in Niuhuang Xiaoyan tab- lets. Methods： An HPLC method was adopted for identification and determination using a Phenomenon Gemini C18 column （250 mm × 4. 6 ram, 5 μm） with a mixture of aeetonitrile and 0.05 mol · L ^-1 ammonium acetate solution （adjusted to pH 4.5 with glacial acetic acid） （40： 60）as the mobile phase at a flow rate of 1 mL ·min^-1. The detection wavelength was set at 618 nm. Meanwhile, the positive results were confirmed by HPLC - MS/MS with ESI ion source. The mixture of aeetonitrile and 5 mmol · L^- 1 ammonium acetate solution （ adjusted to pH 4.5 with gla- cial acetic acid） （40： 60）was used as the mobile phase. The ion at m/z 329 was selected for monitoring and MS/MS analysis. Results： Good separation was obtained in HPLC identification. The detection limit was 0. 03 μg· mL^-1 The selected ion monitoring chromatogram and full scan MS2 spectra of positive samples were consistent with the ref- erence substance of malachite green. For malachite green, the calibration curve was linear in the range of 0.33 - 7.85 μg· mL^-1 and the average recovery was 99. 3%. Conclusion： The proposed method is exclusive,accurate for qualitative detection and quantitative determination of malachite green in Niuhuang Xiaoyan tablets.

关 键 词：牛黄消炎片 孔雀石绿 苯胺绿 碱性绿 化工染料 液相色谱法 液相色谱-质谱联用 染色检测 中成药质量控制 

分 类 号：R286.0[医药卫生—中药学]