止哮平喘颗粒的 HPLC 指纹图谱建立及多指标成分含量测定

李婷; 朱玉燕; 陈骞; 宋畅; 黄志军

doi:10.13748/j.cnki.issn1007-7693.20243628

止哮平喘颗粒的 HPLC 指纹图谱建立及多指标成分含量测定

Establishment of HPLC Fingerprints and Determination of Multi-indicator Components in Zhixiao Pingchuan Granules

摘要

摘要:
目的建立止哮平喘颗粒的HPLC指纹图谱，并对其指标成分进行含量测定，为制剂的质量标准提供参考依据。
方法采用Agilent ZORBAX SB-C₁₈色谱柱(250 mm×4.6 mm，5 μm)，以乙腈-0.1%磷酸为流动相，柱温为25 ℃，流速为1 mL·min⁻¹，进样量为10 μL，芦丁的检测波长为230 nm，其他成分的检测波长为220 nm。采用“中药色谱指纹图谱相似度评价系统(2012版)”建立15批止哮平喘颗粒的HPLC指纹图谱并进行相似度评价，采用SPSS 27.0软件、SIMCA 14.1软件进行聚类分析、主成分分析以及偏最小二乘法判别分析，同时测定芍药苷等8种成分的含量并进行转移率分析。
结果 15批样品的指纹图谱相似度均>0.99。标定了21个峰，指认了10个有效成分，并进行了药材归属。聚类分析及主成分分析结果表示，S1~S4聚为一类，S5~S15聚为另一类。指标成分芍药苷、芦丁、柚皮苷、新橙皮苷、黄芩苷、槲皮素、黄芩素、次野鸢尾黄素的含量分别为2.5883~2.7932、0.7808~1.4214、4.6261~5.2143、5.8996~6.2241、13.4982~14.2202、0.4902~0.5091、0.4514~0.6185、0.1012~0.2056 mg·g⁻¹。药材至饮片，饮片至颗粒的转移率分别为芍药苷83.16%~85.05%、51.69%~54.99%，芦丁79.49%~82.45%、40.80%~54.58%，柚皮苷88.20%~88.62%、65.36%~74.81%，新橙皮苷82.98%~84.01%、70.84%~80.90%，黄芩苷89.62%~95.35%、80.27%~94.42%，槲皮素56.01%~58.34%、46.71%~52.60%，黄芩素85.40%~88.64%、41.27%~49.56%，次野鸢尾黄素73.38%~73.92%、33.24%~38.25%。
结论所建立的止哮平喘颗粒指纹图谱和含量测定方法可靠，同时进行化学模式识别分析，可为制剂的质量标准提供参考依据。

Abstract:
OBJECTIVE To establish the HPLC fingerprints of Zhixiao Pingchuan granules, and to determine the content of its index components, so as to provide a reference basis for the quality standard of the preparation.
METHODS An Agilent ZORBAX SB-C₁₈ column(250 mm×4.6 mm, 5 μm) was used, with acetonitrile-0.1% phosphoric acid as the mobile phase, the column temperature was set at 25 ℃, with the flow rate of 1 mL·min⁻¹, and the injection volume of 10 μL, the detection wavelength of rutin was 230 nm, and that of the other components was 220 nm. The HPLC fingerprints of 15 batches of Zhixiao Pingchuan granules were established and evaluated for similarity using the “Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System(2012 Edition)”, and the cluster analysis, principal component analysis, and partial least squares discriminant analysis were carried out using the SPSS 27.0 software and SIMCA 14.1 software, and the contents of 8 ingredients, including paeoniflorin, were determined and analyzed by transfer rate at the same time.
RESULTS The similarity of the fingerprints of the 15 batches of samples was greater than 0.99. The 21 peaks were calibrated, and 10 active ingredients were identified and attributed to the herbs. The results of cluster analysis and principal component analysis indicated that S1–S4 were clustered into one category, and S5–S15 were clustered into another category. The contents of the index components such as paeoniflorin, rutin, naringin, neohesperidin, baicalin, quercetin, baicalein, and subwild irisin were 2.5883–2.7932, 0.7808–1.4214, 4.6261–5.2143, 5.8996–6.2241, 13.4982–14.2202, 0.4902–0.5091, 0.4514–0.6185, and 0.1012–0.2056 mg·g⁻¹, respectively. The transfer rates of herbs to tablets and tablets to granules were 83.16%–85.05%, 51.69%–54.99% for paeoniflorin, 79.49%–82.45%, 40.80%–54.58% for rutin, 88.20%–88.62%, 65.36%–74.81% for naringin, 82.98%–84.01%, 70.84%–80.90% for neohesperidin, 89.62%–95.35%, 80.27%–94.42% for baicalin, 56.01%–58.34%, 46.71%–52.60% for quercetin, 85.40%–88.64%, 41.27%–49.56% for baicalein, and 73.38%–73.92%, 33.24%–38.25% for irisflorentin.
CONCLUSION The established fingerprints and content determination methods for Zhixiao Pingchuan granules are reliable, and the simultaneous analysis of chemical pattern recognition can provide a reference basis for the quality standard of the preparations.

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