摘要
目的建立快速鉴别海金沙中非法添加柠檬黄的方法。方法采用水试法进行柠檬黄初筛;采用薄层色谱法对柠檬黄进行定性鉴别;采用高效液相色谱法进行验证试验,色谱柱为Agilent Eclipse XDB-C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05 mol/L乙酸铵溶液(梯度洗脱),流速为1.0 m L/min,检测波长为432 nm,柱温为35℃,进样量为10μL。结果药材样品5、样品6溶液呈现与柠檬黄对照品溶液类似且显著的黄色;其薄层色谱图在与柠檬黄对照品色谱图相应位置上显相同的黄色斑点;与柠檬黄对照品的高效液相色谱图保留时间及相应紫外-可见吸收光谱图完全相同,阴性对照无干扰。结论建立的水试法、薄层色谱法和高效液相色谱法,操作简单、快速、准确,适用于快速筛查海金沙中非法添加的柠檬黄,建议申报为海金沙中柠檬黄检查的补充检验方法。
Objective To establish a rapid method for the identification of lemon yellow illegally added in Lygodii Spora.Methods Aqueous solution test was used for lemon yellow preliminary screening.The thin-layer chromatography(TLC)was used for qualitative identification of lemon yellow,and high-performance liquid chromatography(HPLC)was used for the validation test,the chromatographic column was Agilent Eclipse XDB-C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.05 mol/L ammonium acetate solution(gradient elution),the flow rate was 1.0 m L/min,the detection wavelength was 432 nm,the column temperature was 35℃,and the injection volume was 10μL.Results The test solution of sampleⅤandⅥshowed similar and significant yellow color to the control solution of lemon yellow,the TLC chromatograms showed the same yellow spots on the corresponding position of the reference solution of lemon yellow.The retention time of HPLC chromatograms and the corresponding spectrograms of the test solution of sampleⅤandⅥwere the same as those of the reference solution of lemon yellow,and the negative control had no interference.Conclusion The established aqueous solution test,TLC method and HPLC method are simple,rapid and accurate,which are suitable for rapid screening of lemon yellow illegally added in Lygodii Spora.It is recommended to apply for the supplementary inspection method of lemon yellow in Lygodii Spora.
作者
王康
郭舟
张勤
陈建玲
吴竞
WANG Kang;GUO Zhou;ZHANG Qin;CHEN Jianling;WU Jing(Xiangyang Public Inspection and Testing Center,Xiangyang,Hubei,China 441004)
出处
《中国药业》
CAS
2021年第8期55-57,共3页
China Pharmaceuticals
