论文部分内容阅读
目的:建立健儿消食口服液指纹图谱及多指标成分含量测定方法,评价该制剂质量。方法:采用HPLC建立指纹图谱及多指标含量测定方法,并以液质联用法对特征峰进行指认。采用Welch Ultimate C18(4.6 mm×250 mm,5μm)色谱柱,以甲醇为流动相A,0.1%磷酸溶液为流动相B,梯度洗脱(0~60 min,10%A→95%A),流速1.0 m L·min~(-1),检测波长283 nm;采用电喷雾离子源正离子扫描模式,对10个特征峰进行指认。结果:建立了以汉黄芩苷为参照峰的HPLC指纹图谱,并指认了5-羟甲基糠醛、山梨酸钾、橙皮苷、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素7个特征峰。35批样品的相似度值为0.66~1.00,橙皮苷、黄芩苷和汉黄芩苷的含量分别为0.02~0.46、0.73~2.62和0.02~0.45 mg·m L~(-1)。结论:通过研究,发现个别企业存在投料质量差、少投料或工艺过程控制不严等违规生产现象。本研究所建立的指纹图谱及多指标含量测定方法能较好地评价健儿消食口服液的质量,并可为提高该制剂的质量标准,保证产品质量奠定基础。
Objective: To establish the fingerprint of Jian’er Xiaoshi Oral Liquid and the method of determination of multi-index components to evaluate the quality of the preparation. Methods: Fingerprinting and multi-index determination were established by HPLC, and the characteristic peaks were identified by LC / MS. The mobile phase B was eluted with 0.1% phosphoric acid solution (0-60 min, 10% A → 95% A) using a Welch Ultimate C18 column (4.6 mm × 250 mm, 5 μm) The flow rate was 1.0 m L · min ~ (-1) and the detection wavelength was 283 nm. Electron spray ionization positive ion scan mode was used to identify 10 characteristic peaks. Results: The HPLC fingerprinting with baicalin as the reference peak was established and the characteristics of 5-hydroxymethylfurfural, potassium sorbate, hesperidin, baicalin, baicalin, baicalein and wogonin were identified peak. The similarity of 35 batches of samples was 0.66-1.00. The contents of hesperidin, baicalin and baicalin were 0.02-0.46, 0.73-2.62 and 0.02-0.45 mg · m L -1, respectively. Conclusion: Through the research, it is found that some enterprises have the phenomenon of illegal production such as poor feeding quality, less feeding or unscrupulous process control. The fingerprinting and multi-index determination methods established in this study can evaluate the quality of Jian’er Xiaoshi oral liquid better and lay a foundation for improving the quality standard of the preparation and ensuring the product quality.