基于指纹图谱及多指标成分定量的健儿消食口服液质量评价  

Quality evaluation of Jianerxiaoshi mixture by HPLC fingerprint and multi-component quantitative analysis

作　　者：程巧鸳 唐登峰 马临科 陈碧莲 祝明 

机构地区：[1]浙江省食品药品检验研究院,杭州310052

出　　处：《药物分析杂志》2016年第1期148-154,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(No.81303213)

摘　　要：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 HPLC fingerprints and multi-component quantitative analysis of Jianerxiaoshi mixture, so as to evaluate its quality. Methods： The fingerprint and quantitative analysis were performed by HPLC. The characteristic peaks were identified by LC-MS. The separation was developed on a Welch Ultimate column （ 4.6 mm × 250 mm, 5 μm ） with a gradient elution （ 0-60 min, 10% A → 95% A ） of methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B at a flow rate of 1.0 mL· min^-1, and the detection wavelength was 283 nm. Ten characteristic peaks in the fingerprints were identified with applying electrospray ionization （ ESI ） source in the positive ion mode. Results： The fingerprint of Jianerxiaoshi mixture was established with wogonoside as the reference peak. Seven characteristic peaks in the fingerprint were identified as 5-hydroxymethyl furfural, potassium sorbate, hesperidin, baicalin, wogonoside, baicalein and wogonin. The similarity values of 35 batches of samples ranged from 0.66 to 1.00. The content of hesperidin, baicalin, wogonoside in different batches ranged from 0.02 to 0.46 mg＂ mL-1, from 0.73 to 2.62 mg· mL^-1 and from 0.02 to 0.45 mg ·mL^-1, respectively. Conclusion： Some illegal production phenomena were found with raw materials of poor quality or less amount, and lax process control, etc. The method of fingerprint and multi- component quantitative analysis established in this study could be applied in the quality control of Jianerxiaoshi mixture. This study also provided a basis to improve the quality standard and ensure the quality of the preparation.

关 键 词：健儿消食口服液 中成药指纹图谱 多指标含量测定 相似度分析 橙皮苷 黄芩苷 汉黄芩苷 液相色谱一质谱联用法 

分 类 号：R917[医药卫生—药物分析学]