超高效液相色谱-串联质谱法测定白芷中51种禁用农药的残留量

将白芷药材粉碎至通过孔径为(250±9.9)μm的网筛,并称取此白芷粉末样品2.00g于聚丙烯管中与水10mL混匀,再加入含1%(体积分数)乙酸的乙腈10.0mL,涡旋1min后加入无水硫酸镁4g和乙酸钠1g,剧烈振荡3min,离心5min,取其上清液5.0mL置于已盛有无水硫酸镁900mg、N-丙基乙二胺(PSA)450mg和硅胶300mg的净化管中,剧烈振荡5min使净化完全,离心5min。移取上清液3.0mL于40℃水浴中减压蒸缩至近干。加入50μg·L^-1的磷酸三苯酯内标溶液300μL,加入乙腈定容至1.0mL,经0.20μm滤膜过滤,取其滤液,按仪器工作条件进行超高效液相色谱-串联质谱法分析。选用Eclipse Plus C18色谱柱和以不同比例的(A)含10mmol·L^-1甲酸铵的0.1%(体积分数)甲酸溶液和(B)乙腈的混合液为流动相,按梯度洗脱程序对白芷中可能残留的51种禁用农药进行色谱分离,并在电喷雾离子源正、负离子(ESI+和ESI-)电离方式和动态多反应监测(dMRM)模式条件下进行串联质谱法测定。采用基质匹配标准曲线法定量。51种农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,并测得其检出限(3S/N)为0.3~5.0μg·kg^-1。标准加入法回收试验的结果显示,其中大部分农药的回收率在71%以上,测定值的相对标准偏差(n=6)均小于20%。按此方法分析了70批白芷样品,共检出16种农药,其中甲拌磷亚砜的检出率达95%,最高检出量为15.2μg·kg^-1;甲拌磷砜和毒死蜱的检出率均为10%,最高检出量依次为3.5,45.0μg·kg^-1,其余13种农药的检出率均低于5%,且检出量均较低。     

密闭微波辅助萃取当归粉中的阿魏酸

利用密闭微波样品制备系统(具有压力控制部件),对当归中的有效成分阿魏酸的萃取进行研究,比较了密闭微波萃取同超声波萃取和索氏萃取阿魏酸提取率的差异.结果表明:微波萃取与其他两种萃取方法相比,具有速度快和萃取率高的特点.并得到了阿魏酸提取的最佳条件:微波功率为400 W,萃取剂为90%的乙醇(体积分数),固-液比为1∶15,微波辐射为240 s,当归粒径为75μm.     

中药川白芷化学成分的研究

中药川白芷为伞形科当归属杭白芷 (Ａｎｇｅｌｉｃａｄａｈｕｒｉｃａ (Ｆｉｓｃｈ .ｅｘＨｏｆｆｍ .)Ｂｅｎｔｈ .ｅｔＨｏｏｋ .ｃｖｈａｎｇ ｂａｉｚｈｉＨｏｒｔ)的干燥根。川白芷为我国传统中药 ,主治头疼、鼻炎、癣症等疾病。现代药理实验表明白芷中所含的呋南香豆素具有平喘、降压、抗菌、解痉、光敏、活化交感系激素等多种药理作用[1] 。已有文献对白芷的化学成分进行了研究 ,发现白芷中主要含香豆素成分[2～ 4] 。四川遂宁产川白芷为道地白芷 ,其药性好 ,为进一步研究其活性成分 ,本文对遂宁产川白芷进行化学成分研究。共分离、…     

表面活性剂增敏2.5次微分极谱测定香豆素

拟定了表面活性剂增敏、2 .5次微分极谱测定香豆素的方法。在含 6.0× 10 -6 mol·L-13 氯 2 羟丙基 三甲基氯化铵的 0 .1mol·L-1KH2 PO4 Na2 HPO4 (pH 6.8)缓冲液中 ,香豆素还原波 [峰电位Ep=- 1.60V(vs .SCE) ]的 2 .5次微分极谱峰峰电流e″p 与其浓度在 4 .0× 10 -7～ 6.0× 10 -5mol·L-1范围内呈良好线性关系 (r =0 .9998,n =10 ) ,检出限为 1.2× 10 -7mol·L-1。 13次平行测量 8.0× 10 -6 mol·L-1香豆素的峰电流 ,RSD为 1.5 %。该方法可用于中药白芷中香豆素的直接测定     

第4代航天育种白芷的FTIR分析

针对植物航天育种变异大的特点,利用傅里叶变换红外光谱(FTIR)结合二阶导数谱对第4代航天育种白芷与地面组白芷从整体上对主要组分进行测定和对比分析。结果表明:太空白芷主要活性成分香豆素类组分(1 741cm-1)含量增加,蛋白质(1 459,1 419cm-1)和脂肪(930cm-1)组分含量略有增加;而淀粉、膳食纤维(1 152,1 105,1 080,1 050cm-1)的含量大幅度降低。二阶导数谱中峰强差异更明显,1 279cm-1处揭示出太空白芷含有胺类组分。航天育种有利于选育出变异幅度大的特异质白芷新品种。     

Metabolic study of Angelica dahurica extracts using a reusable liver microsomal nanobioreactor by liquid chromatography–mass spectrometry

Highly active and recoverable nanobioreactors prepared by immobilizing rat liver microsomes on magnetic nanoparticles (LMMNPs) were utilized in metabolic study of Angelica dahurica extracts. Five metabolites were detected in the incubation solution of the extracts and LMMNPs, which were identified by means of HPLC‐MS as trans‐imperatorin hydroxylate (M1), cis‐imperatorin hydroxylate (M2), imperatorin epoxide (M3), trans‐isoimperatorin hydroxylate (M1′) and cis‐isoimperatorin hydroxylate (speculated M2′). Compared with the metabolisms of imperatorin and isoimperatorin, it was found that the five metabolites were all transformed from these two major compounds present in the plant. Since no study on isoimperatorin metabolism by liver microsomal enzyme system has been reported so far, its metabolites (M1′ and M3′) were isolated by preparative HPLC for structure elucidation by ¹H‐NMR and MS² analysis. M3′ was identified as isoimperatorin epoxide, which is a new compound as far as its chemical structure is concerned. However, interestingly, M3′ was not detected in the metabolism of the whole plant extract. In addition, a study with known chemical inhibitors on individual isozymes of the microsomal enzyme family revealed that CYP1A2 is involved in metabolisms of both isoimperatorin and imperatorin, and CYP3A4 only in that of isoimperatorin. Copyright © 2015 John Wiley & Sons, Ltd.     

气相色谱-质谱法测定当归粉、当归原药材中的邻苯二甲酸二丁酯

建立了气相色谱-质谱法测定当归粉和当归原药材中邻苯二甲酸二丁酯（DBP）的方法。在国家标准的基础上,通过单因素试验,优化了提取方法和提取溶剂,确定了以正己烷为提取剂从水中液液萃取的方法。方法学试验结果表明,DBP浓度在0．01～1．00μg／mL范围内与色谱峰面积呈良好的线性关关系,线性相关系数r^2=0．9995,检出限为0．05μg／g（全扫描）,不同水平的加标回收率在90％～100％之间,测定结果的相对标准偏差小于5％（n=3）。该方法适合当归粉和当归原药材中DBP的日常检测。     

Triterpenoids and Iridoid Glycosides from Gentiana dahurica

One new and six known pentacyclic triterpenoids, 1 and 4 – 9 , resp., along with two new and three known iridoid glycosides, 2 and 3 , and 10 – 12 , resp., were isolated from the roots of Gentiana dahurica (‘Qin‐Jiao’). The new structures were elucidated by means of spectroscopic and chemical methods as 1β,2α,3α,24‐tetrahydroxyursa‐12,20(30)‐dien‐28‐oic acid ( 1 ), 6′‐O‐acetylgentiopicroside ( 2 ), and 3′‐acetylgentiopicroside ( 3 ). Isolated compounds were tested for their cytotoxicity against the MCF‐7 human breast cancer cell line using the MTT assay. Among them, triterpenoids 2α,3β,24‐trihydroxyurs‐12‐en‐28‐oic acid ( 6 ) and 3β,24‐dihydroxyurs‐12‐en‐28‐oic acid ( 9 ) were found to have moderate cytotoxic effects with IC₅₀ values of 20.9 and 21.7 μg/ml, respectively. Additionally, the chemotaxonomic significance of the identified secondary metabolites is briefly discussed.     

浓缩当归丸的提取工艺研究

采用索氏提取法提取浓缩当归丸的有效成分阿魏酸，同时用正交分析法对提取溶剂种类、用量及提取时间进行考察，最后以高效液相色谱法(HPLC)测定阿魏酸的含量，从而筛选出最佳提取工艺．结果显示：选用60mLV甲醇：V甲酸=95：5的混合液作为提取溶剂．预先浸泡24h，再索氏提取3h，得到浓缩当归丸的有效成分阿魏酸的含量最高．     

达乌里秦艽化学元素特征及其与环境关系

应用全谱直读等离子体发射光谱法（ICP—AES）对不同居群达乌里秦艽（Gentiana dahurica Fischer）中15种元素含量进行了测定,通过聚类分析和主成分分析探讨了其化学元素特征及与生态环境的关系,为深入认识该药材的元素特征及其功效提供参考。结果表明,达乌里秦艽药用部位元素含量较丰富,以大量元素K,Ca和Mg含量较高。不同居群元素含量水平显示出地理分布差异特点;且各元素之间具一定的协调促进或拮抗作用,这种作用在聚类分析中再次得到证明;主成分分析的结果表明,其元素特征可用“代谢增强”作用因子和“酶活促进”作用因子来体现。海拔对两个因子有正向促进作用;经纬度则对前者具负向影响,对后者具正向影响。