WU Wenping,HE Minyou,WU Shuzhen,et al.Study on UPLC Fingerprints and QAMS of Mume Fols Dispensing Granules[J].zhongguo zhongyiyao xinxi zazhi,2020,27(8):86-91.[doi:10.3969/j.issn.1005-5304.201911564]
梅花配方颗粒超高效液相色谱指纹图谱及一测多评法研究
- Title:
- Study on UPLC Fingerprints and QAMS of Mume Fols Dispensing Granules
- 文章编号:
- 1005-5304(2020)08-0086-06
- Keywords:
- Mume Fols dispensing granules; fingerprints; QAMS; hyperoside; isoquercitrin; chlorogenic acid; rutin
- 分类号:
- R284.1
- 文献标志码:
- A
- 摘要:
- 目的 建立梅花配方颗粒超高效液相色谱指纹图谱,并应用一测多评法同时测定梅花配方颗粒中绿原酸、金丝桃苷、异槲皮苷、芦丁含量,为其质量控制提供依据。方法 采用Waters BEH C18色谱柱(2.1 mm×150 mm,1.7 μm),以甲醇-0.1%磷酸为流动相进行梯度洗脱,流速0.25 mL/min,检测波长355 nm,柱温40 ℃,进样量1 μL,测定11批梅花配方颗粒的指纹图谱,建立指纹图谱共有模式。采用一测多评法,以金丝桃苷为内参物,通过相对校正因子测定绿原酸、异槲皮苷、芦丁含量,同时采用外标法测定11批梅花配方颗粒中4个指标成分的含量,比较计算值与实测值的差异,验证一测多评法的准确性。结果 11 批梅花配方颗粒指纹图谱标定了13个色谱峰,指认了其中6个化学成分。11批样品指纹图谱与对照指纹图谱的相似度均大于0.99。建立相对校正因子重现性良好,采用相对校正因子计算的含量值与实测值之间无明显差异。结论 本研究建立的测定方法简便快捷、准确、重复性良好,可为梅花配方颗粒的质量控制和评价提供依据。
- Abstract:
- Objective To establish UPLC fingerprints of Mume Fols dispensing granules, and to determine the contents of chlorogenic acid, hypericin, isoquercetin, rutin in Mume Fols dispensing granules by quantitative analysis of multi-components by single marker ( QAMS); To provide references for its quality control. Methods The analysis was carried out on a Waters BEH C18 column (2.1 mm × 150 mm, 1.7 μm) with the mobile phase of methanol - 0.1% phosphoric acid at a flow rate of 0.25 mL/min in gradient elution mode ; the detection wavelength was 355 nm , and the column temperature was 40 ℃. The injection volume was 1 μL. The common mode of UPLC fingerprint was established by determined of 11 batches of Mume Fols dispensing granules. A QAMS method was developed. With hypericin as the internal reference, the contents of chlorogenic acid, isoquercetin and rutin were measured by relative correction factor. External standard method was performed to determine 4 index components in 11 batches of Mume Fols dispensing granules. The difference between the calculated value and the measured value was compared to verify the accuracy of QAMS. Results 13 common peaks were marked in the fingerprints of 11 batches of Mume Fols dispensing granules and 6 of them were identified. The similarities between the fingerprints of samples and control were all greater than 0.99. The established relative correction factor had good reproducibility, and there was no significant difference between the content value calculated using the relative correction factor and the measured value. Conclusion The method is simple, rapid, accurate and repeatable, which can provide references for quality control and evaluation of Mume Fols dispensing granules.
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备注/Memo
基金项目:广东省省级科技计划项目(2018B030323004);广东省中药配方颗粒工程实验室(2018年)
更新日期/Last Update:
2020-07-20