双黄连胶囊HPLC指纹图谱的不确定度和可靠度研究

The Uncertainty and Reliability of HPLC Fingerprints of Shuanghuanglian Capsule

目的建立中药指纹图谱不确定度和可靠度评价方法并评价双黄连胶囊(Shuanghuanglian Capsule,SHLC)HPLC指纹图谱的不确定度和可靠度。方法采用RP-HPLC法,以黄芩苷(baicalin,BCL)为参照物峰,确定53个共有指纹峰,建立了SHLC-HPLC指纹图谱并用系统指纹法评价12批SHLC质量,针对SHLC-HPLC对照指纹图谱和12批样品指纹图谱进行不确定度和可靠度评价。结果 SHLC-HPLC对照指纹图谱的定性可靠度和定量可靠度分别大于0.981和0.938,表明对照指纹图谱反映的化学指纹数量和含量分布比例以及整体含量的可靠性很高。S5,S7,S8和S9的定性和定量不确定度较高,可靠度很低,表明其反映的化学指纹数量分布和含量分布与整体含量的可信性较低。虽然S4质量为6级,其定性和定量可靠度分别为0.979和0.961,表明将S4评价为6级的结论可靠度高于S6。结论所建立的不确定度评价方法能准确反映中药指纹图谱的变动性,可靠度评价方法可准确评价对照指纹图谱和单批指纹图谱所表征的定性和定量信息的可靠程度。

Objective To develop an evaluation method of uncertainty and reliability for traditional Chinese medicine fingerprints and assess the uncertainty and reliability of Shuanghuanglian Capsule（SHLC） of High Performance Liquid Chromatographic（HPLC） fingerprints. Methods The chromatographic fingerprints（CFP） were determined by reversed-phase（RP） HPLC,in which 53 common peaks were marked by choosing baicalin（BCL） peaks as the reference peak,in which the systematic quantified fingerprint method was applied to evaluate the quality of 12 batches of SHLC,meanwhile,the uncertainty and reliability of SHLC referential fingerprint（RFP） and 12 batch sample fingerprints were evaluated. Results The qualitative reliability and quantitative reliability of SHLC-HPLC-RFP were more than 0.981 and 0.938 respectively,it showed that the reliability of the chemical fingerprint quantity,the distribution proportion and the overall content that reflected by RFP were very high.The qualitative uncertainty and quantitative uncertainty of S5,S7,S8 and S9 were all high,i.e.the reliability were all low,which indicated their reliability of the chemical fingerprint quantity,the distribution proportion and the overall content were lower.S4 belonged to 6 quality grade,its qualitative reliability and quantitative reliability were 0.979 and 0.961 respectively,so we could make sure the reliability of conclusion was high. Conclusion The evaluation method of uncertainty can accurately reflect the variances in traditional Chinese medicine fingerprints,and that of reliability would exactly estimate the degree of reliability of qualitative and quantitative information included in both RFP and each sample fingerprint.