黄芪多糖注射液中非法添加林可霉素检查方法的研究

Determination Methods of Lincomycin Illegally Adulterated into the Astragalus Polysaccharides Injection by TLC/HPLC-PDAD/LC-MS

关键词:  林可霉素  黄芪多糖注射液  薄层色谱  高效液相色谱  质谱

Key words:  Lincomycin  the astragalus polysaccharides injection  TLC  HPLC  MS

摘要:

建立检测黄芪多糖注射液中非法添加的检查方法。采用薄层色谱法初筛，再以HPLC-PDAD法检查，最后用LC-MS法确证。薄层色谱法初筛出的在黄芪多糖注射液中非法添加林可霉素的样品，用HPLC-PDAD法检测，液相色谱条件: 采用Atlantis? T 3（十八烷基硅烷键合硅胶，4.6mm i.d×250mm，5μm），流动相为0.02 mol/L的磷酸氢二铵-乙腈（70:30），流速为1.0 mL/min，检测波长：194nm；最后用LC-MS法进行确证。结合薄层色谱、高效液相色谱光谱图以及质谱的分子离子峰等方面信息，证明该样品中确实非法添加了林可霉素，其中HPLC-PDAD法平均回收率均在97.8%，RSD为1.4%；检出限均6μg/mL。该检测方法准确可靠，可用于黄芪多糖注射液中非法添加林可霉素的检测。

Abstract:

The study was aimed to establish TLC and HPLC-PDAD methods for determination of lincomycin illegally adulterated into the astragalus polysaccharides injection, and then identified by LC-MS. The method of TLC was used as a pretest, then the methods of HPLC-PDAD and LC-MS were used to identify lincomycin illegally adulterated into the astragalus polysaccharides injection. HPLC-PDAD was performed on a column of Atlantis? T 3 (4.6 mm×250 mm, 5 μm) at 194nm. The mobile phase consisted of a mixture of a solution of 0.02 mol/L ammonium phosphate dibasic and acetonitrile（70:30）at a flow rate of 1.0 mL/min. The average recovery was 97.8% with RSD was 1.4%. The limit of detection of the method was 6μg/mL. It has been proved that there was lincomycin illegally adulterated into the astragalus polysaccharides injection based on the data of the spots in the chromatogram of TLC, the retention time of HPLC including ultraviolet spectra and the molecular ion mass spectra. The method is accurate and reliable, and can be used to lincomycin illegally adulterated into the astragalus polysaccharides injection.