目的 建立高效液相色譜一測(cè)多評(píng)（QAMS）法同時(shí)測(cè)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(nèi)酯A、藁本內(nèi)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(guò)灰色關(guān)聯(lián)度分析法對(duì)13種成分含量檢測(cè)結(jié)果進(jìn)行分析評(píng)價(jià)。方法 采用Shimadzu C₁₈色譜柱；以乙腈-0.1%磷酸為流動(dòng)相梯度洗脫；檢測(cè)波長(zhǎng)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(nèi)酯A、藁本內(nèi)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(biāo)法（ESM）測(cè)定13種成分的含量。以葛根素為內(nèi)參物質(zhì)，分別計(jì)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(nèi)酯A、藁本內(nèi)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(duì)校正因子（f），并計(jì)算上述12種成分的含量，比較ESM和QAMS法檢測(cè)結(jié)果的差異，驗(yàn)證一測(cè)多評(píng)法的準(zhǔn)確性和可行性。基于灰色關(guān)聯(lián)度分析不同批次頸痛顆粒中13種成分QAMS法含量檢測(cè)數(shù)據(jù)，對(duì)15批次頸痛顆粒質(zhì)量進(jìn)行綜合評(píng)價(jià)。結(jié)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(nèi)酯A、藁本內(nèi)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(nèi)線性關(guān)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(jì)算值和ESM實(shí)測(cè)值之間無(wú)明顯差異?；疑P(guān)聯(lián)度分析結(jié)果顯示15批次頸痛顆粒相對(duì)關(guān)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(zhì)量差異。結(jié)論 QAMS多指標(biāo)成分定量控制聯(lián)合灰色關(guān)聯(lián)度分析法操作便捷、結(jié)果準(zhǔn)確，可用于頸痛顆粒的綜合質(zhì)量評(píng)價(jià)。

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.

R284.1

國(guó)家中醫(yī)藥管理局全國(guó)中藥特色技術(shù)傳承人才培訓(xùn)項(xiàng)目（國(guó)中醫(yī)藥人教函〔2018〕204號(hào)）；國(guó)家中醫(yī)藥管理局全國(guó)名老中醫(yī)藥專家工作室建設(shè)項(xiàng)目（國(guó)中醫(yī)藥人教函〔2022〕75號(hào)）