西黄丸和活血止痛散中乳香及非法添加松香的薄层色谱鉴别

Identification of Olibanum and Illegally Adulterated Colophony in Xihuang Pills and Huoxue Zhitong Powders by Thin Layer Chromatography

目的建立薄层色谱鉴别方法检测西黄丸和活血止痛散中的乳香药材及非法添加的松香。方法样品经甲醇超声提取,点样于硅胶GF254薄层板上,以甲苯-乙酸乙酯-庚烷-无水甲酸(8∶2∶1∶0.3)为展开剂展开,先置紫外灯(254nm和366nm)下检视,再喷以茴香醛试液,并于105℃加热至条斑清晰,日光下再次检视。结果紫外光灯(254nm)及日光下,西黄丸和活血止痛散与乳香对照药材的薄层指纹图谱一致,使用对照品识别了11-羰基-β-乙酰乳香酸(AKBA)、11-羰基-β-乳香酸(KBA)、β-乳香酸(β-BA)和β-乙酰乳香酸(β-ABA);紫外光灯(366nm)下,活血止痛散可见与当归对照药材一致的条斑。紫外光灯(254nm)下,某些西黄丸色谱中可见松香中松香酸的暗条斑。结论该法简便、专属,适用于西黄丸和活血止痛散薄层色谱鉴别和质量控制。

Objective To establish a method for identification of olibanum and illegally adulterated colophony in Xihuang pills and Huoxue zhitong powders by thin-layer chromatography （TLC）. Methods The samples were extracted by ultrasonic with menthol. Chromatography was performed on a silica gel 60F254 TLC plate, using toluene： ethyl acetate： heptanes： anhydrous formic acid （8 ： 2 ： 1 ： 0. 3） as the mobile phase, examined in the ultraviolet lights at 254 nm and 366 nm, then in the white light after being derived with anisaldehyde test solution and heated at 105℃ to clarify the band. Results The TLC fingerprints of Xihuang pills and Huoxue zhitong powders corresponded to those of the reference material of olibanum by which acetyl-ll-keto-β-boswellic acid （AKBA）, 11-keto-β-boswellic acid （KBA）, β- boswellic acid （β-BA）, and acetyl-β-boswellic acid （β-ABA） were identified. In the ultraviolet light at 366 nm, Huoxue zhitong powders showed bands that corresponded to the reference drug of Angelicae Sinensis Radix. In the ultraviolet light at 254 nm, certain bands of Xihuang pills were identified to the abietic acid reference substance. Conclusion The method is simple, and specific, which can be used for TLC identification and quality control of Xihuang pills and Huoxue Zhitong powders.