分子排阻色谱法检测双黄连注射液中的高分子杂质

Determinationof high molecular mass impurities in Shuanghuanglian injection by molecular exclusion chromatography

目的分子排阻色谱法考察双黄连注射液中高分子杂质。方法采用分子排阻色谱法测定了3个厂家6批双黄连注射液,用TSKk-GEL G2000SWxL色谱柱,以乙腈-水-三氟乙酸(体积比40∶60∶0.07)为流动相,流速为0.5 mL·min-1,柱温为30℃,二极管阵列检测器,检测波长为214 nm。结果相对分子质量对数与出峰时间呈良好的线性关系(r=0.996 8),相对分子质量对照品(人胰岛素)检出限为0.386 mg·L-1,6批双黄连注射液中均未检出高分子物质,加速稳定性试验检测相对分子质量3 108>Mr≥1 638杂质的含量稳定。结论国内的双黄连注射液质量稳定,在加速稳定性试验中无高分子物质聚合产生,作者建立的检测方法可用于双黄连注射液中高分子杂质的检查。

Objective To establish a molecular exclusion chromatography method for determination of high molecular mass impurities in Shuanghuanglian injection （traditional Chinese medicine）. Methods A molecu- lar exclusion chromatography was used to determine a total of 6 samples, the separation was performed in TSKk-GEL G2000SWxL column with mobile phase of acetonitrile-water-trifluoroacetic acid （ V： V： V = 40：60：0. 07）. The flow rate was 0. 5 mL.min^-1 and the column temperature was 35.L-1,detected by diode array detector,and the detection wavelength was set at 214 nm. Results A good linear correlation was ob- served in the molecular weight standard curve of polypeptide polymer material （ r = 0. 996 8 ）, Molecular weight control products detection limit was 0. 386 mg. L^-1, the high molecular mass impurities were not de- tected in the 6 batch of Shuanghuanglian injection. The contents of molecular weight （3 108 〉 Mr≥ 1 638 ） impurities are stable after accelerated stability test. Conclusions The high molecular mass impurities are not detected in domestic Shuanghuanglian injection, and no polymers are observed after accelerated stability test. The method is simple ,rapid and reliable for determination of high molecular mass impurities in Shuanghuan- glian injection.