摘要
目的:建市检测抗风湿类中成药中非法掺入萘普生、吲哚美辛的专属性方法。方法:采用液相色谱-电喷雾质谱联用法。液相色谱:色谱柱为 Agilent C_(18)柱(150 mm×4.6 mm,5 μm),流动相为0.02 moL·L^(-1)醋酸铵-1%醋酸溶液-甲醇(32:3:65),流速0.4 mL·min^(-1);柱温30℃。质谱:电喷雾电离源(ESI)负离子检测;质荷比范围 m/z 100～400,干燥气温度350℃;干燥气流速10 L·min^(-1);干燥气压力276 kPa;源电压为5 kV。通过相对分子质量、一级及二级质谱碎片信息、液相色谱保留时间和紫外光潜四方面的信息,对抗风湿类中成药的提取液中非法掺入的萘普生、吲哚美辛进行定性鉴别。结果:6批抗风湿类中药,3批检出掺有萘普牛,其中2批检出同时掺有吲哚美辛。结论:该方法选择性强,灵敏度高,可作为分析检测抗风湿类中成药中萘普生、吲哚美辛的有效方法,可用于分析鉴定中成药非法添加西药成分的打假工作。
Objective： To develop a specific method for the identification of naproxen and indometacin illegally added into Chinese medicine preparations. Methods ： The liquid chromatography - ion trap mass spectrometry method was used. LC：Agilent C18 column （150 mm ×4.6 mm,5 μm） ,the mobile phase consisting of 0.02 mol·L^-1 ammonium acetate - 1% acetic acid - methanol （ 32 ： 3 ： 65 ） , a flow rate of 0.4 mL ·min^-1, column temperature 30 ℃. MS ： negative electrospray ionization （ ESI - ） and two scan modes including full scan MS and full scan MS - MS,the scanning range of 100 -400 m/z,the drying gas temperature of 350 ℃ ,the drying gas flow rate of 10 L ·min^ -1 , the drying gas pressure of 276 kPa, the ionization voltage of 5 kV. The obtained pseudomolecular ions, fragment ions uv -spectrogram and retention time were used to identify the two drugs by comparison with those of reference substances. Results：Three formulations were detected illegally adulterated by naproxen and two of them were simultaneously detected illegally adulterated by indometacin. Conclusion：The method is specific, sensitive and accurate, thus it can be used to determinate the Chinese Traditional Medicines,illegally adulterated by the anti -rheumatism drugs.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第8期1276-1279,共4页
Chinese Journal of Pharmaceutical Analysis
