基于柱效指数监测的双波长定量比率指纹图谱评价朱砂安神丸

Evaluating Zhusha Anshen pills by quantity ratio fi ngerprints monitored by the column effi ciency index of chromatographic fi ngerprints

目的建立色谱指纹图谱柱效指数模型,用以检测定量指纹图谱的变化。方法用高效液相色谱二极管阵列检测器同时测定12批朱砂安神丸(ZSASP)在203 nm和286 nm指纹谱(NFP)和比率指纹图谱(ROFP),分别以均值法整合同波长下指纹图谱,最后进行双波长指纹图谱的二次均值整合,计算双波长指纹图谱柱效指数并进行比较。结果以小檗碱(BBR)为参照物峰,确定57(203 nm)和50(286 nm)个共有指纹峰,建立了双波长ZSASP-HPLC指纹图谱和比率指纹图谱。首先将同波长下的NFP和ROFP进行均值整合,之后进行双波长二次均值整合鉴定出S1、S4、S5、S6、S9和S10质量极好(1级),S2、S3、S11和S12质量很好(2级),S7和S8质量次(7级)。在203 nm,S4、S5、S6、S9柱效指数较高,而在286 nm下四者柱效指数较低造成两者差值很大,S8呈现上述反变化过程造成较大差异值。结论色谱指纹图谱柱效指数能监测中药定量指纹图谱的柱效关联分离度后的变化情况,因此柱效指数标志着信号均化性和分离度均化性以及峰宽变动情况。

Objective To set up the column effi ciency index of chromatographic fi ngerprints, and to monitor the chang of quantity fi ngerprints. Methods A high performance liquid chromatography(HPLC) coupled with diode array detector(DAD) was employed to determine the normal fi ngerprints(NFPs) and the ratio fi ngerprints(ROFPs) of 12 batches of Zhusha Anshen pills(ZSASPs) at 203 nm and 286 nm wavelengths simultaneously. They were averaged under the same wavelength respectively, and then averaged again by dual wavelengths. Meanwhile the column effi ciency index was calculated. Results We marked 57(203 nm) and 50(286 nm) co-possessing peaks by choosing berbine(BBR) peak as the referential peak, so the quantity NFPs and quantity ROFPs of the 12 batches of ZSASPs at 203 nm and 286 nm wavelengths were simultaneously developed. After averaging both NFPs and ROFPs under the same wavelengths twice, we again averaged them under dual wavelengths and identifi ed that the quality of S1, S4, S5, S6, S9 and S10(G1) was best, that of S2, S3, S11 and S12 was better(G2), while that of S7 and S8 was defective(G7). Big difference was shown in dual wavelengths for the column effi ciency index of chromatographic fi ngerprints of S4, S5, S6 and S9 because they had much higher values under 203 nm but very low values under 286 nm, and the opposite true for S8. Conclusion The column effi ciency index of chromatographic fi ngerprint can monitor the change of column effi cacy associated with the resolution. Therefore it refl ects the leveling degree of both the fi ngerprint signals and resolutions as well as the peak widths changes.