目的 構(gòu)建芍藥甘草湯基準樣品HPLC指紋圖譜及11種成分定量測定方法，同時建立大類成分總黃酮、總苷、總酚、總多糖的UV含量測定手段，全面評價基準樣品的質(zhì)量，為芍藥甘草湯基準樣品質(zhì)量控制提供依據(jù)。方法 運用高效液相色譜法（HPLC）構(gòu)建芍藥甘草湯基準樣品的HPLC指紋圖譜，并同步實現(xiàn)11種指標成分的定量測定，同時，結(jié)合化學計量學方法，明確芍藥甘草湯基準樣品的差異性特征成分；借助紫外-可見分光光度法，對芍藥甘草湯基準樣品中的總黃酮、總苷、總酚、總多糖含量進行檢測分析，在此基礎上，深入剖析11個有效成分在總黃酮、總苷、總酚3個大類成分中的占比情況，從而達成對芍藥甘草湯基準樣品質(zhì)量的系統(tǒng)性、全面性評價。結(jié)果 建立了17批芍藥甘草湯基準樣品指紋圖譜，相似度均大于0.9，標定了13個共有峰，指認了其中11個色譜峰信息；17批芍藥甘草湯基準樣品中沒食子酸、芍藥內(nèi)酯苷、芍藥苷、芹糖甘草苷、甘草苷、苯甲酸、1,2,3,4,6-五沒食子酰葡萄糖、異甘草素、甘草素、異甘草苷、甘草酸銨的質(zhì)量分數(shù)分別為2.72～4.92、4.82～19.44、29.68～40.98、2.94～6.10、5.47～7.90、1.31～3.44、0.83～1.10、0.67～0.96、0.78～1.52、0.12～0.23、10.16～20.29 mg·g^-1，芍藥內(nèi)酯苷、芍藥苷、甘草酸銨為區(qū)分不同批次芍藥甘草湯基準樣品的差異性標志物；17批基準樣品總黃酮質(zhì)量分數(shù)為2.25%～3.45%、總苷質(zhì)量分數(shù)為9.40%～14.18%、總酚質(zhì)量分數(shù)為0.97%～2.19%、總多糖質(zhì)量分數(shù)為45.44%～59.47%，大類成分總質(zhì)量分數(shù)為62.64%～75.97%；11個定量指標在黃酮類、酚酸類、苷類成分占比分別為44.20%～54.19%、32.95%～59.76%、43.11%～61.70%。結(jié)論 建立的指紋圖譜及質(zhì)量分數(shù)測定方法可靠，重復性及準確性良好，結(jié)合化學計量學篩選的質(zhì)量差異物，可為后續(xù)質(zhì)量評價研究提供依據(jù)。

Objective HPLC fingerprint chromatogram of the benchmark sample of the Shaoyao Gancao Decoction and the quantitative determination method of 11 components were established. Meanwhile, the UV content determination methods of the major components such as total flavonoids, total glycosides, total phenols and total polysaccharides were developed to comprehensively evaluate the quality of the benchmark sample and provide a basis for the quality control of the benchmark sample of the Shaoyao Gancao Decoction.Methods The HPLC fingerprint chromatogram of the benchmark sample of the Shaoyao Gancao Decoction was constructed by HPLC, and the quantitative determination of 11 index components was simultaneously achieved. In addition, the characteristic components of the benchmark sample of the Shaoyao Gancao Decoction were identified by chemometrics. The contents of total flavonoids, total glycosides, total phenols and total polysaccharides in the benchmark sample of the Shaoyao Gancao Decoction were detected by UV spectrophotometry. On this basis, the proportion of 11 effective components in the three major components of total flavonoids, total glycosides and total phenols was analyzed in depth to achieve a systematic and comprehensive evaluation of the quality of the benchmark sample of the Shaoyao Gancao Decoction.Results The HPLC fingerprint chromatograms of 17 batches of benchmark samples of the Shaoyao Gancao Decoction were established, with similarity greater than 0.9. Thirteen common peaks were identified, and the information of 11 chromatographic peaks was recognized. The mass fractions of gallic acid, paeoniflorin, paeonol, apioside, liquiritin, benzoic acid, 1, 2, 3, 4, 6-pentagalloyl glucose, isoliquiritigenin, liquiritigenin, isoliquiritin and ammonium glycyrrhizinate in 17 batches of benchmark samples of the Shaoyao Gancao Decoction were 2.72—4.92, 4.82—19.44, 29.68—40.98, 2.94—6.10, 5.47—7.90, 1.31—3.44, 0.83—1.10, 0.67—0.96, 0.78—1.52, 0.12—0.23 and 10.16—20.29 mg·g^-1, respectively. Paeoniflorin, paeonol and ammonium glycyrrhizinate were the differential markers for distinguishing different batches of benchmark samples of the Shaoyao Gancao Decoction. The contents of total flavonoids, total glycosides, total phenols and total polysaccharides in 17 batches of benchmark samples were 2.25%—3.45%, 9.40%—14.18%, 0.97%—2.19% and 45.44%—59.47%, respectively. The total content of major components was 62.64%—75.97%. The proportions of 11 quantitative indicators in flavonoids, phenolic acids and glycosides were 44.20%—54.19%, 32.95%—59.76% and 43.11%—61.70%, respectively.Conclusion The established fingerprint chromatogram and content determination method were reliable, with good repeatability and accuracy. Combined with the quality difference substances screened by chemometrics, it can provide a basis for subsequent quality evaluation research.

R283.6

國家工信部產(chǎn)業(yè)基礎再造和制造業(yè)高質(zhì)量發(fā)展專項（2440STCZB2614）