基于UPLC-Q-TOF-MS/MS结合响应面法与主成分分析优化肠炎合剂Ⅱ提取工艺  

Optimization of the Extraction Process of Changyan HejiⅡBased on UPLC-Q-TOF-MS/MS Combined with Response Surface Method and Principal Component Analysis

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作  者:汪树林 商晶[2] 刘文君[2] 蔡泽荣 钱梦雨 胡晓欣 曹亮[2] 王振中[2] 肖伟[1,2] WANG Shulin;SHANG Jing;LIU Wenjun;CAI Zerong;QIAN Mengyu;HU Xiaoxin;CAO Liang;WANG Zhenzhong;XIAO Wei(State Key Laboratory of Technologies for Chinese Medicine Pharmaceutical Process Control and Intelligent Manufacture(Jiangsu Kanion Pharmaceutical Co.,Ltd.&Nanjing University of Chinese Medicine),Nanjing 210000,China;Jiangsu Kanion Pharmaceutical Co.,Ltd,Lianyungang 222000,China;School of Traditional Chinese Pharmacy,China Pharmaceutical University,Nanjing 211198,China)

机构地区:[1]中药制药过程控制与智能制造技术全国重点实验室(江苏康缘药业股份有限公司/南京中医药大学),江苏南京210000 [2]江苏康缘药业股份有限公司,江苏连云港222000 [3]中国药科大学中药学院,江苏南京211198

出  处:《南京中医药大学学报》2025年第4期501-512,共12页Journal of Nanjing University of Traditional Chinese Medicine

基  金:江苏省基础研究计划自然科学基金-前沿引领技术基础研究专项(BK20232014)。

摘  要:目的基于UPLC-Q-TOF-MS/MS技术结合响应面分析构建肠炎合剂Ⅱ提取工艺方法,并对其提取工艺进行优化。方法通过UPLC-Q-TOF-MS/MS技术对肠炎合剂Ⅱ中化学成分进行定性分析,并挑选出质谱响应度有较好线性关系的化学成分为工艺考察指标;利用Box-Behnken设计对提取工艺参数(加水量、提取时间及浸泡时间)进行考察;通过主成分分析(Principal component analysis,PCA)得到综合评分,并以综合得分结合响应面分析确定最优工艺。结果通过定性分析从肠炎合剂Ⅱ中推测和鉴定了110个成分,包括有机酸2种、黄酮类82种、萜类化合物13种、生物碱类13种,基于定性分析结果,通过UPLC-Q-TOF-MS/MS结合Masshunter质谱数据分析软件导出48个具有良好线性关系的指标成分质谱响应度,进行PCA并计算综合得分,以综合得分为指标进行响应面分析,综合响应面预测结果及生产实际得到的最优提取工艺为:浸泡45 min,溶剂倍量8倍,提取2次,每次120 min。结论为中药复方提取工艺的考察提供了一种新思路,为中药复方开发拓展一种新方法。OBJECTIVE To establish a extraction process of Changyan HejiⅡ(CYHJ-Ⅱ)based on UPLC-Q-TOF-MS/MS technology combined with response surface analysis,and to optimize the extraction process.METHODS The chemical components in CYHJ-Ⅱwere qualitatively analyzed by UPLC-Q-TOF-MS/MS technology,and the chemical components with good linear relationship in mass spectrometry response were selected as process investigation indicators;the extraction process parameters(water addition amount,extraction time and soaking time)were investigated by Box-Behnken design;the comprehensive score was obtained by principal component analysis(PCA),and the optimal process was determined by the comprehensive score combined with response surface analysis.RESULTS Through qualitative analysis,110 components were inferred and identified from CYHJ-Ⅱ,including 2 organic acids,82 flavonoids,13 terpenoids,and 13 alkaloids.Based on the results of qualitative analysis,48 index components with good linear relationships were derived by UPLC-Q-TOF-MS/MS combined with Masshunter mass spectrometry data analysis software.PCA was performed and the comprehensive score was calculated.Response surface analysis was performed with the comprehensive score as an indicator.The optimal extraction process obtained by combining the response surface prediction results and actual production was:soaking for 45 min,8 times the amount of solvent,2 extractions,each time for 120 min.CONCLUSION This study provides a new idea for the investigation of the extraction process of traditional Chinese medicine compound prescriptions and expands a new method for the development of traditional Chinese medicine compound prescriptions.

关 键 词:提取工艺 Box-Behnken设计-响应面法 主成分分析 葛根素 甘草酸 木香烃内酯 芍药苷 

分 类 号:R284.1[医药卫生—中药学]

 

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