止痛止痒类中成药中非法添加化学药物的快速鉴定方法

Rapid analysis of analgesic and antipruritic illegally added in herb preparations

目的建立止痛止痒类中成药制剂非法添加8种化学药品(醋酸泼尼松、醋酸氟轻松、醋酸地塞米松、醋酸可的松、倍他米松、泼尼松、双氯芬酸钠、吲哚美辛)的快速检测方法。方法采用薄层色谱法(TLC)快速初筛中药制剂中可能添加成分,高效液相色谱对筛查出的疑似样品进行进一步分析,其色谱柱为Sun Fire C18(250 mm×4.6mm,5μm),流动相A为0.5%HAc溶液-四氢呋喃(100∶1),流动相B为乙腈-0.5%HAc溶液-四氢呋喃(80∶20∶1),梯度洗脱;柱温25℃,检测波长254 nm。结果清新百合紫苏胶囊中添加了醋酸泼尼松;腰间盘突出止痛贴和风湿骨痛贴中添加了双氯芬酸钠。结论本测定方法采用TLC和HPLC法结合的方式可用于筛查中药制剂中非法添加微量糖皮质激素和镇痛药成分。

AIM To develop a rapid analysis for screening eight kinds of analgesic and antipruritic illegally added （prednisone acetate, fluocinolone acetonide, dexamethasone acetate, cortisone acetate, betamethasone, prednisone, diclofenac sodium, and indomethacin） in herb preparations. METHODS Firstly, TLC method was used to find the possibility of the eight possible additives in the test preparations, then the suspicious samples were investigated by HPLC method to characterize and assay possible additives. SunFire C18 （250 mm×4.6mm,5μm） column was adopted with mobile phase A consisted of 0. 5% HAc-tetrahydrofunan （100 ： 1 ）, mobile phase B acetonitrile- 0. 5% HAc-tetrahydrofunan （80 ： 20 ： 1 ） in gradient elution manner. Column temperature was maintained at 25℃, and detection wavelength was set at 254 nm. RESULTS Prednisone acetate was found in Qingxin Baihe Zisu Capsules, and diclofenac sodium was detected to be illegally added in Yaojianpan Tuchu Zhi- tong Plaster and Fengshi Gutong Plaster. CONCLUSION The combination of TLC and HPLC has been proved effective in treating the traces of analgesic and glucocorticoids illegally adulterated.