[關鍵詞]
[摘要]
目的 建立高效液相色譜一測多評(QAMS)法同時測定頸痛顆粒中三七皂苷R1、人參皂苷Rg1、人參皂苷Rb1、3'-羥基葛根素、葛根素、3'-甲氧基葛根素、洋川芎內酯A、藁本內酯、延胡索乙素、去氫紫堇堿、紫堇堿、羌活醇和異歐前胡素含量,并通過灰色關聯(lián)度分析法對13種成分含量檢測結果進行分析評價。方法 采用Shimadzu C18色譜柱;以乙腈-0.1%磷酸為流動相梯度洗脫;檢測波長為203 nm(三七皂苷R1、人參皂苷Rg1和人參皂苷Rb1)、280 nm(3'-羥基葛根素、葛根素、3'-甲氧基葛根素、洋川芎內酯A、藁本內酯、延胡索乙素、去氫紫堇堿和紫堇堿)和315 nm(羌活醇和異歐前胡素);采用外標法(ESM)測定13種成分的含量。以葛根素為內參物質,分別計算其與三七皂苷R1、人參皂苷Rg1、人參皂苷Rb1、3'-羥基葛根素、3'-甲氧基葛根素、洋川芎內酯A、藁本內酯、延胡索乙素、去氫紫堇堿、紫堇堿、羌活醇和異歐前胡素的相對校正因子(f),并計算上述12種成分的含量,比較ESM和QAMS法檢測結果的差異,驗證一測多評法的準確性和可行性?;诨疑P聯(lián)度分析不同批次頸痛顆粒中13種成分QAMS法含量檢測數(shù)據(jù),對15批次頸痛顆粒質量進行綜合評價。結果 三七皂苷R1、人參皂苷Rg1、人參皂苷Rb1、3'-羥基葛根素、葛根素、3'-甲氧基葛根素、洋川芎內酯A、藁本內酯、延胡索乙素、去氫紫堇堿、紫堇堿、羌活醇和異歐前胡素分別在各自范圍內線性關系良好(r≥0.999 2),平均加樣回收率(n=9)在96.86%~100.37%(RSD≤1.65%)。所建立的f耐用性良好,HPLC-QAMS法計算值和ESM實測值之間無明顯差異?;疑P聯(lián)度分析結果顯示15批次頸痛顆粒相對關聯(lián)度在0.332 4~0.600 4,表明頸痛顆粒批次間呈現(xiàn)一定質量差異。結論 QAMS多指標成分定量控制聯(lián)合灰色關聯(lián)度分析法操作便捷、結果準確,可用于頸痛顆粒的綜合質量評價。
[Key word]
[Abstract]
Objective To establish a HPLC-QAMS method for simultaneous determination of notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1, 3'-hydroxy puerarin, puerarin, 3'-methoxy puerarin, senkyunolide A, ligustilide, tetrahydropalmatine, dehydrocorydaline, corydaline, notopterol and isoimperatorin in Jingtong Granules, and to analyze and evaluate the content detecting results of 13 components by grey relational analysis. Methods The chromatographic column Shimadzu C18 was used. And using acetonitrile-0.1% phosphoric acid as mobile phase with gradient elution. The detection wavelength were 203 nm for notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1, 280 nm for 3'-hydroxy puerarin, puerarin, 3'-methoxy puerarin, senkyunolide A, ligustilide, tetrahydropalmatine, dehydrocorydaline, corydaline and 315 nm for notopterol and isoimperatorin. The contents of 13 components were determined by external standard method (ESM). Taking puerarin as internal standard substance, the relative correlation factor (f) of notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1, 3'-hydroxy puerarin, 3'-methoxy puerarin, senkyunolide A, ligustilide, tetrahydropalmatine, dehydrocorydaline, corydaline, notopterol and isoimperatorin was calculated, and the contents of 12 components were calculated. The differences between the content detecting results by ESM and HPLC-QAMS method were compared. Based on the grey relational degree, the HPLC-QAMS method conent detection data of 13 component of different batches of Jingtong Granules were analyzed, and the sample of 15 batches of Jingtong Granules was comprehensively quality evaluated. Results Notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1, 3'-hydroxy puerarin, puerarin, 3'-methoxy puerarin, senkyunolide A, ligustilide, tetrahydropalmatine, dehydrocorydaline, corydaline, notopterol and isoimperatorin had good linearity in their respective ranges (r ≥ 0.999 2). The average recoveries of the 13 components (n = 9) were between 96.86%—100.37% with the relative standard deviations less than 1.65%. The established RCF had good durability, and the results calculated with HPLC-QAMS method were consistent with the results by the ESM. The results of grey correlation analysis showed that the relative correlation degree of 15 batches of Jingtong Granules was 0.332 4—0.600 4, indicating that there was a certain quality difference between batches of Jingtong Granules. Conclusion HPLC-QAMS multi-index component quantitative control combined with grey relational analysis is convenient and accurate, and can be used for the comprehensive quality evaluation of Jingtong Granules.
[中圖分類號]
R284.1
[基金項目]
國家中醫(yī)藥管理局全國中藥特色技術傳承人才培訓項目(國中醫(yī)藥人教函〔2018〕204號);國家中醫(yī)藥管理局全國名老中醫(yī)藥專家工作室建設項目(國中醫(yī)藥人教函〔2022〕75號)