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UPLC/Q Exactive MS快速测定食蟹猴体内黄藤素的血药浓度 被引量:1
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作者 张培培 崔佳丽 +2 位作者 周艺佳 刘红斌 柯瑾 《昆明医科大学学报》 CAS 2020年第6期39-45,共7页
目的建立UPLC-Q Exactive-MS快速检测食蟹猴血浆中黄藤素的方法。方法采用Ulti Mate 3000系列高效液相色谱仪和Q Exactive四极杆-静电场轨道阱高分辨质谱系统检测。猴含药血浆采用乙腈沉淀蛋白,盐酸小檗碱为内标,蛋白沉淀后用乙腈稀释... 目的建立UPLC-Q Exactive-MS快速检测食蟹猴血浆中黄藤素的方法。方法采用Ulti Mate 3000系列高效液相色谱仪和Q Exactive四极杆-静电场轨道阱高分辨质谱系统检测。猴含药血浆采用乙腈沉淀蛋白,盐酸小檗碱为内标,蛋白沉淀后用乙腈稀释并测定,色谱柱为Hypersil GOLD Dim C18 column (100 mm×2.1 mm,1.9μm),乙腈-0.1%甲酸水为流动相,梯度洗脱,流速0.3m L/min,柱温30℃,电喷雾正离子化(ESI+),选择性离子扫描模式(t-SIM):黄藤素,[M-Cl]+,m/z 352.15433;内标盐酸小檗碱,[M-Cl]+,m/z 336.123 03。分辨率70000,自动增益控制(AGC)和离子注入时间(IT)分别设为5e4和200 ms;isolation window设为4.0 m/z。喷雾气为氮气,碰撞气为高纯氮气。结果黄藤素在105.0~8 200μg/L (进样样品溶液浓度为0.262 5~20.50μg/L)浓度范围内线性关系良好(线性方程为Y=0.001 188 51C-0.000 042 206 6,r=0.999 6,权重1/C2),最低定量限为105.0μg/L,日内与日间精密度均小于4.06%,目标物和内标基质效应因子为91.71~97.74%(n=5),未处理血浆样品于室温放置约1 d、-20℃放置1 d/10 d/35 d、-20℃放置35 d后室温冻融2次稳定性良好。结论建立的LC-MS分析检测方法线性范围宽、分析时间短、准确度好、灵敏度高、特异性强,适于黄藤素药代及毒代动力学分析检测。 展开更多
关键词 黄藤素 UPLC-Q exactive-ms 快速测定
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Effect of processing cycles on the composition of Polygonatum cyrtonema Hua during nine-steam-nine-bask processing 被引量:8
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作者 Xiangjie Yao Zeyuan Deng +1 位作者 Hongyan Li Bing Zhang 《Food Bioscience》 SCIE 2022年第6期777-787,共11页
Nine-steam-nine-bask is a traditional method for the processing of polygonatum cyrtonema Hua,which is a homology plant of medicine and food,but why is nine cycles of steam-bask needed is still not clear.This study aim... Nine-steam-nine-bask is a traditional method for the processing of polygonatum cyrtonema Hua,which is a homology plant of medicine and food,but why is nine cycles of steam-bask needed is still not clear.This study aims to investigate the changes of functional components caused by each processing cycle and optimize the best number of processing cycles for the preparation of polygonatum.It was found that the content of total polysaccharide decreased with the increase of processing cycles and stabled at about 5.2 g/100 g,which was reduced by 45.81%compared with raw polygonatum(10.899 g/100 g,p<0.05).However,the contents of saponins,phenols and flavonoids as well as the in vitro antioxidant activity of polygonatum showed an increasing trend,which had slight fluctuations after the fourth processing cycle.Besides,a total of 48 volatile components and 221 non-volatile components were identified by GC-MS and UPLC-Q Exactive MS/MS,respectively.Among them,2,3-butanediol was the major numb-taste component in polygonatum which could be eliminated by processing and 113 differential non-volatile components were screened.To sum up,the four processing cycles could be sufficient for edible and medicine without the need of nine-steam-nine-bask. 展开更多
关键词 POLYGONATUM Nine-steam-nine-bask processing Functional components content Antioxidant activity HS-GC-MS UPLC-Q exactive-ms/MS
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