延平胶囊中非法添加化学药品的检测方法研究

目的建立TLC结合HPLC法检查保健食品延平胶囊中非法添加的化学药品氢氯噻嗪、苯磺酸氨氯地平。方法采用硅胶GF254板,甲苯-醋酸乙酯-异丙醇-浓氨试液(12:3:3:0.2)为展开剂,在254nm下检视;采用Lichrospher C18柱,流动相:磷酸盐缓冲液(取磷酸二氢钾13.6g,加水80mL溶解后,加磷酸调节pH值至3.0,再加水至100mL)-甲醇-水(4:25:71),流速:1.0mL.min-1,检测波长:225nm,柱温:35℃。结果延平胶囊非法掺入化学药品氢氯噻嗪、苯磺酸氨氯地平在254nm下显明显的斑点。通过HPLC-DAD法进一步验证了结果。结论本法操作简便,结果可靠,可用于检测延平胶囊中非法添加的化学药品氢氯噻嗪、苯磺酸氨氯地平。

Study on Detection Method of Hydrochlorothiazide and Amlodipine Besylate Illegally Added in Yanping Capsules

Objective To establish a method for detection of hydrochlorothiazide and amlodipine besylate illegally added in Yanping Capsules by TLC combined with HPLC.Methods Silica gel（GF254）TLC was used,a mixture of methylbenzene-ethyl acetate-isopropanol-Ammonium hydroxide（12∶3∶3∶0.2） as developer,detecting under 254nm.Lichrospher C18 column was used,and the mobile phase consisted of phosphate buff solution（Dissolve 13.6 g of potassium dihydrogen phosphate in 80mL of water,adjust the pH value to 3.0 with phosphoric acid,and dilute with water to 100mL）-methanol-water（4∶25∶71）.Flow rate was 1.0mL ·min-1;detective wavelength was 225nm;column temperature was 35℃.Results The hydrochlorothiazide and amlodipine besylate illegally added in Yanping Capsules were displayed obvious dots under 254nm.Then they were verified by HPLC-DAD.Conclusion The method is simple and accurate.It can be used for detection of hydrochlorothiazide and amlodipine besylate illegally added in Yanping Capsules.