色谱特征指纹定量法和多标定量指纹法评价血府逐瘀丸质量

Evaluation of the quality of Xuefu Zhuyu pills by quantified characteristic fingerprint method and quantified multi-marker fingerprint method

目的研究系统指纹定量法（SQFM）评价血府逐瘀丸（XFZYP）相对特征指纹图谱时误差变动和校正方法进行研究。方法采用反相高效液相色谱法,以Agilent Poroshell 120 SB-C18柱（150 mm×4.6 mm,2.7μm）,流速0.5 m L·min-1,紫外检测波长203 nm,柱温（35.0±0.1）℃,进样量5μL为条件,采集24批XFZYPs的HPLC指纹图谱（NFP）,对其变换得到统一化指纹图谱（UFP）和相对特征指纹图谱（RCFP）,以各对照指纹图谱（RFP）为标准用SQFM评价24批XFZYPs质量情况,阐述其Pm差异性和校正方法。单标定量指纹法可将所有指纹峰的含量用单标含量表观标示,双标和多标用折合质量标示。结果确定37个共有指纹峰,用单标RCFP和UFP评价结果的宏定性相似度不发生改变;宏定量相似度的误差都能用参照峰校正因子进行校正消除,而双标结果的误差较大。质量极好的XFZYPs同时要满足单标和双标定量相似度合格,共有S14、S18、S20~S23等6批样品可作为标准制剂。结论色谱相对特征指纹图谱均能对样品进行准确地定性定量评价,其能有效地使用国家药典委员会关于指纹图谱的相对特征技术参数。

Objective To study the variance errors and correcting methods of relative characteristic fingerprint evaluated by systematically quantified fingerprint method（SQFM） when evaluating the quality of Xuefu Zhuyu pills（XFZYPs）. Methods The column was an Agilent Poroshell 120 SB-C18（150 mm×4.6 mm, 2.7 μm） at 0.5 m L·min- 1, the detection wavelength was 203 nm, the column temperature was（35.0±0.1） ℃ and the injection volume was 5 μL. A total of 24 batches of XFZYPs HPLC chromatographic fingerprints were determined to establish a normal fingerprint（NFP）, the unified fingerprint（ UFP） and relative characteristic fingerprint（RCFP）. The quality of 24 batches of XFZYPs was evaluated by SQFM with each reference fingerprint（RFP） as the standard, and the distinctions within Pm and correction methods were elucidated. The content of all fingerprint peaks was marked equivalently by the quantified one marker fingerprint method（Q1FM）, quantified two marker fingerprint method（Q2FM） and quantified multimarker fingerprint method（Qm FM）. Results Totally 37 co-possessing peaks were marked and the results of Q1 FM and UFP showed that the macro qualitative similarity did not change, while the errors were thoroughly eliminated by the correction factor of the reference peak. The errors of Q2 FM were much bigger because of bi-errors. The best XFZYPs must meet the requirement of Q1 FM and Q2 FM quantitative similarity at the same time. S14, S18, and S20-S23 were selected as the standard preparations. Conclusion The sample can be accurately evaluated qualitatively and quantitatively by relative chromatographic characteristic fingerprints which can effectively use the relative technical parameters defined by state pharmacopoeia commission.