用LC/MS和AA等方法检测确定中成药豨莶风湿片中掺有双氯芬酸钠

Determination of Diclofenac Sodium in Xixian Fengshi Tablets by LC/MS and AA etc

目的:建立有效的方法确定中成药豨莶风湿片中的化学镇痛药双氯芬酸钠。方法:采用TLC、HPLC、LC/MS及AA等分析手段。TLC条件:采用硅胶GF254薄层板上,以乙酸乙酯-三氯甲烷-冰醋酸(25∶25∶0.2)为展开剂,展开后,晾干,置紫外光灯(254nm)下检视;HPLC条件:采用迪马C18柱(4.6×150mm,5μm)色谱柱,流动相为甲醇-0.02mol·L-1醋酸钠溶液(用冰醋酸调节pH值至3.7)(65∶35),流速为1.0ml.min-1,检测采用DAD及紫外测定波长282nm,柱温为35℃;LC/MS条件:流动相为乙腈-0.2%醋酸溶液(梯度洗脱),采用ESI离子源,正离子方式检测,毛细管温度300℃,鞘气压力70;AA条件:空气-乙炔火焰,检测波长589.0nm(钠离子测定)和766.5nm(钾离子测定)。结果:通过四种色谱和光谱方法的联合检测,逐步证明所测豨莶风湿片中含有化学镇痛药为双氯芬酸钠。结论:本手段能有效地打击假药。

Objective： Establishing an effective method to determine Diclofenac Sodium in Xixian Fengshi Tablets. Methods：TLC,HPLC,LC/MS and AA methods were used. The method of TLC was developed by using thin-layer of GF2s, in a mixture of butanol,triehloror, lethane ,and glacial acetic acid （25 ： 25 ： 0.2）. The method of HPLC was developed by using a Dikma C18 as the column with the mobile phase of methanol-0. 02mol·L^-1（using acetic acid to adjust to pH 3.7）（65 ： 35）, and a flow rate was set at 1.0mol·L^-1. The column temperature was 35℃. Detection was performed with DAD detector and UV detector at 282nm. The method of LC/NS was carried out by using the ion source of ESI with positive modes. The capillary temperature was 300℃. Result：Dielofenae Sodium which was exited in Xixian Fengshi Tablets can be determined by using the above four methods. Conclusion：This method can effectively beat the bogus medidne.