比率指纹图谱定量评价柏子养心丸质量

Quality of Baizi Yangxin pills by quantified ratio HPLC fingerprints

目的以样品指纹峰面积xi和对照指纹峰面积yi之比ri=xi/yi对保留时间作图得到比率指纹图谱(ROFP),以样品指纹向量XR=(x1/y1,x2/y2,···,xn/yn)=(r1,r2,···,rn)→和对照指纹图谱(标准制剂指纹)向量YR=(1,1,···,1)=(100%,100%,···,100%)→为基础建立中药比率指纹定量法(QRFM)以定性定量控制中药质量。方法用高效液相色谱二极管阵列检测器同时测定12批柏子养心丸228、286和326 nm指纹谱,以均值法整合三波长下指纹图谱和ROFP的评价结果,并与正常指纹图谱(NFP)评价结果进行比较。结果以绿原酸(CGA)为参照物峰,确定56(228 nm)、53(286 nm)和45(326 nm)个共有指纹峰,建立了三波长BZYXP-HPLC指纹图谱和ROFP。首先将三波长下得到的NFP和ROFP进行均值整合,之后再对NFP和ROFP进行二次均值整合鉴定出S11(1级)质量极好,S2、S3、S4、S6和S10质量很好(2级);S1、S5、S8和S9质量好(3级);S7质量次(7级);S12质量劣(8级)。结论 ROFP各指纹量值一致使其评价结果更准确和更客观,但奇异峰比值易引起误差。QRFM对中药复杂轮廓化学成分的整体定量更客观和更准确。基于中药标准制剂控制模式,以定量指纹图谱为基础和使用QRFM是中药质量一致性和均一性控制的重要方法。

Objective To obtain the ratio fi ngerprints（ROFP） by plotting the ratio of the sample＇s peak area（xi） to the referential peak area（yi）（ ri=xi/yi） versus the retention time（tR, min）, and to establish the quantifi ed ratio fi ngerprint method（QRFM） based on both the sample fi ngerprint vector XR=（x1/y1, x2/y2, …, xn/yn）=（r1, r2, …, rn）→and the referential fi ngerprint vector YR=（1, 1,…, 1）=（100%, 100%, …, 100%）→so as to qualitatively and quantitatively control the quality of traditional Chinese medicine（TCM）. Methods A high performance liquid chromatography（HPLC） method coupled with diode array detector（DAD） was performed to obtain the normal fingerprints（NFP） of 12 batches of Baizi Yangxin pills at 228, 286 and 326 nm wavelength simultaneously. The NFP and ROFP evaluation of the 3 wavelength was integrated by the average method, in which the NFP results and the ROFP results were compared. Results We marked 56（228 nm）, 53（286 nm） and 45（326 nm） co-possessing peaks respectively by choosing chlorogenic acid（CGA） peak as the referential peak, so the normal NFPs and ROFPs of the 12 batches of Baizi Yangxin pills at 228, 286 and 326 nm wavelengths were simultaneously developed. Before two average method in NFPs and ROFPs under 3 wavelengths, we employed the average method within them to identify that the quality： S11（G1） was the best, that of S2, S3, S4, S6 and S10 was better（G2）, that of S1, S5, S8 and S9 was good（G3）, that of S7 was inferior（G7）, and that of S12 was defective（G8）, which showed QRFM was superior to systematically quantifi ed fi ngerprint method（SQFM） in accuracy. Conclusion The ROFP evaluation is more accurate and more objective than NFPs. QRFM can qualitatively and quantitatively evaluate the complex TCM system of diverse chemical components more objectively and more accurately. The overall quantitative quality control of TCM can be better and more reliable and more reasonable based on the quality control mode of TCM standard preparation.