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

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WelchUltimate 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 mL·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·mL^-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,5μm)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 multicomponent 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.

[1] 中国药典2010年版. 一部[S]. 2010:999 ChP 2010. Vol Ⅰ[S]. 2010:999
[2] 李静,阿孜古丽·阿布都逊,高晓黎. 健儿消食口服液的薄层色谱鉴别研究[J]. 新疆医科大学学报, 2007, 30(4):358 LI J, AZIGULI·A, GAO XL. TLC research of Jianerxiaoshi mixture[J]. J Xinjiang Med Univ, 2007, 30(4):358
[3] 李静,焦胜春,彭曦,等. HPLC法测定健儿消食口服液中橙皮苷和黄芩苷的含量[J]. 中成药, 2009, 31(10):1638 LI J, JIAO SC, PENG X, et al. Assay of hesperidin and bacalin in Jianerxiaoshi mixture by HPLC[J]. Chin Tradit Pat Med, 2009, 31(10):1638
[4] 张洁玫,罗丽娟,陈美清. HPLC法测定健儿消食口服液中黄芩苷的含量[J]. 中草药, 2001, 32(7):611 ZHANG JM,LUO LJ,CHEN MQ. Assay of baicalin in Jianerxiaoshi mixture by HPLC[J]. Chin Tradit Herb Drugs,2001,32(7):611
[5] 戚进,余伯阳. 中药质量评价新模式——" 谱效整合指纹谱" 研究进展[J]. 中国天然药物, 2010, 8(3):171 QI J, YU BY. A new methodology for the quality evaluation of traditional Chinese medicine-integrated spectrum-effect fingerprint research[J]. Chin J Nat Med, 2010, 8(3):171
[6] 李强,杜思邈,张忠亮,中药指纹图谱技术进展及未来发展方向展望[J]. 中草药, 2013, 44(22):3095 LI Q,DU SM,ZHANG ZL,et al. Progress in fingerprint technology on Chinese materia medica and prospect of its future development[J]. Chin Tradit Herb Drugs, 2013, 44(22):3095