减肥中成药中添加西布曲明西药成分的检测

Determination of Sibutramine Added in the Diet Pills of Traditional Chinese Medicine

目的 建立检测减肥类中成药中可能添加西药西布曲明的定性、定量方法。方法 随机抽查市场上销售的3种减肥药，采用TLC及LC-MS联用技术定性鉴别，HPLC外标法定量．结果 硅胶HF254薄层板上，以氯仿-甲醇（8：1）为展开刺，改良碘化铋钾溶液显色，供试品与对照品及阳性对照比较，呈现相同的橘红色斑点，Rf值为0．65。流动相：甲醇-水（80：20，pH4.5），流速1．0mL·min^-1，柱后分流，0．4mL·min^-1进质谱仪；ESI（＋）离子源，扫描范围m／z100～400，干燥气流速8．00L·min^-1，干燥气温度350℃，雾化气压2.1×10^5Pa；借助于液相色谱-质谱联用仪的质量色谱图方式识别和确认西布曲明的保留时间，并获取其对应峰位的质谱图，供试品与对照品质谱图对比，碎片离子峰匹配因子达到0．999，检出西布曲明。HPLC定量分析，通过改变流动相及调整流速，样品中西布曲明作为定量峰与相邻干扰峰有较好的分离度，3种减肥中成药中的西布曲明分别在30～350，10～180，10～250mg·L^-1内具有良好的线性关系（r分别为0.9996，0．9990，0．9993，R=7）。结论 本法简便、快速、分离效果好、精密度、准确度高，可用于中成药复杂的化学环境中添加西布曲明的定性、定量分析。

OBJECTIVE To establish a method for detecting Sibutramine illegally added in the complicated diet pills of traditional Chinese Medicine already.METHODS Three diet pills were chosen in random. They were determined by TCL, HPLC and LC-MS. The extemal standardization method was used for the quantitative analysis. RESULTS By means of TLC, followed by developing on silica gel HF254percolated plates with a mixture of chloroform-methanol （8： 1） as fluent, potassium bismuth iodide was used as visualization reagent, they all had a similar Rf value（0.65） and the color is red-orange. The mobile phase consisted of methanol-water（80 ： 20, pH 4.5） with a flow rate of 0.4 mL·min^-1, ESI（ ＋ ）ion source, scan range m/z 100- 400, dry gas 8.00 L·min^-1, dry temp 350 ℃ and nbulizer 2.1 × 10^5Pa. Compared the mass spectrogram of sibutramine standard with sample, the match factor of fragment ion peaks was to 0.999. The sibutramine was also detected by HPLC.Their calibration curves were linear in concentration ranges of 30 ～ 350,10 ～180 and 10～ 250 mg·L^- 1 （ r = 0.999 6,0.999 0 and 0.999 3, n = 7）. CONCLUSION The method is simple, rapid and reliable for determining sibutranine in the complicated diet pills, which is used as a qualitative and quantitative method.