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UPLC-MS/MS法分析旋覆花蜜炙前后化学成分的变化
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| 篇名： | UPLC-MS/MS法分析旋覆花蜜炙前后化学成分的变化 |
| TITLE： | Variations of Chemical Components in Inula japonica by UPLC-MS/MS before and after Honey-frying |
| 摘要： | 目的：比较旋覆花蜜炙前后的化学成分差异。方法：采用超高效液相色谱-串联质谱技术（UPLC-MS/MS）。色谱柱为WatersACQUITYUPLCBEHC18，流动相为0.1％甲酸溶液-乙腈（梯度洗脱），流速为0.3mL/min，柱温为30℃，进样量为5µL。采用电喷雾离子源，以正离子模式扫描，一级质谱扫描范围为m/z70～1050，二级质谱扫描范围为m/z50～1050，归一化碰撞能量为40、60eV，质谱图类型为峰形图，鞘气流速为35arb，辅助气流速为10arb，喷雾电压为3.80kV，透镜电压为50V，加热温度为350℃，毛细管温度为350℃。采用QualBrowser4.1.39.1软件并参考在线高分辨数据库mzCloud、中药成分高分辨质谱本地数据库OTCML，同时结合相关文献对化合物进行鉴定。采用SIMCA14.1软件进行主成分分析（PCA）、正交偏最小二乘法-判别分析（OPLS-DA），以变量重要性投影（VIP）值大于1为标准筛选旋覆花蜜炙前后的差异性成分。结果：从旋覆花及其蜜炙品中共鉴定出29个共有化学成分，包括1-咖啡酰奎宁酸、绿原酸、3，5-二咖啡酰奎宁酸等5个酚酸类成分，槲皮素、木犀草素、狭叶依瓦菊素等12个黄酮类成分，以及1-O-乙酰旋覆花内酯、二大花旋覆花内酯B、1-O-乙酰基-6-O-异丁酰基大花旋覆花内酯等12个倍半萜内酯类成分。PCA结果显示，旋覆花与蜜旋覆花分别位于得分图的两侧。OPLS-DA结果显示，有7个成分的VIP值大于1，分别为峰19（大花旋覆花素）、峰6（槲皮万寿菊苷）、峰1（1-咖啡酰奎宁酸）、峰21（紫花牡荆素）、峰20（tomentosin）、峰13（菠叶素）、峰3（瑞香素）。结论：经蜜炙后，旋覆花的化学成分含量有所改变，且均有一定程度的降低。大花旋覆花素、槲皮万寿菊苷、1-咖啡酰奎宁酸、tomentosin、紫花牡荆素、菠叶素、瑞香素可能为旋覆花及其蜜炙品的差异性成分。 |
| ABSTRACT： | OBJECTIVE：To compare the c hemical components differences of Inula japonica before and after honey-frying. METHODS：UPLC-MS/MS method was adopted. The determination was performed on Waters ACQUITY UPLC BEH C 18 column with mobile phase consisted of 0.1％ formic acid-acetonitrile （gradient elution ）at the flow rate of 0.3 mL/min. The column temperature was set at 30 ℃，and sample size was 5 µL. The electrospray ion source was scanned by positive ion mode. The first order mass spectrometry scanning range was m/z 70-1 050，the second order mass spectrometry scanning range was m/z 50-1 050， and the normalized collision energy was 40，60 eV ；mass spectrum type was the peak figure ，the flow rate of sheath gas was 35 arb，the auxiliary airflow speed was 10 arb，the spray voltage was 3.80 kV，the S-lens voltage was 50 V，the heating temperature was 350 ℃，and the capillary temperature was 350 ℃. The components were identified by Qual Browser 4.1.39.1 software， referring to the online high-resolution database mzCloud and local database OTCML of high-resolution mass spectrometry of TCM ， and combined with relevant literature. The principal component analysis （PCA）and orthogonal partial least squared-discriminant analysis（OPLS-DA）of I. japonica before and after honey-fried were performed by using SIMCA 14.1 statistical software ，and variable importance projection （VIP）value greater than 1 was used as the standard to screen the differential components before and after honey-frying. RESULTS ：A total of 29 common chemical components were identified from I. japonica and honey-fried I. japonica，including 5 phenolic acids as 1-caffeoylquinic acid ，chlorogenic acid and 3，5-dicaffeoylquinic acid ，12 flavonoids as quercetin，luteolin and evamectin ，as well as 12 sesquiterpene lactones as 1-O-acetylinula diester ，inula bicolor lactone B and 1-O-acetyl-6-O-isobutyryl inulin. The results of PCA showed that I. japonica and honey-fried I. japonica were located on both sides of the score diagram respectively. The results of OPLS-DA showed that the VIP values of 7 components were greater than 1，which were peak 19（britanin），peak 6（quercetagitrin），peak 1（1-caffeoylquinic acid ），peak 21（vitexicarpin），peak 20（tomentosin）， peak 13（spinacetin）and peak 3（daphnetin）. CONCLUSIONS ：After honey-fried ，the content of chemical components of I. japonica changed and decreased to a certain extent. Britanin ，quercetagitrin，1-caffeoylquinic acid ，tomentosin，vitexicarpin， spinacetin and daphnetin may be the differential components of I. japonica and honey-fried I. japonica . |
| 期刊： | 2021年第32卷第20期 |
| 作者： | 吕渭升，位翠杰，潘晓君，杨文惠，何民友，陈向东，孙冬梅，魏梅，李振雨 |
| AUTHORS： | LYU Weisheng，WEI Cuijie， PAN Xiaojun，YANG Wenhui，HE Minyou，CHEN Xiangdong，SUN Dongmei，WEI Mei，LI Zhenyu |
| 关键字： | 旋覆花；蜜旋覆花；超高效液相色谱-串联质谱法；主成分分析；正交偏最小二乘法-判别分析；化学成分 |
| KEYWORDS： | Inula japonica ；Honey-fried Inula japonica ；UPLC-MS/MS；PCA；OPLS-DA；Chemical components |
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