黄芪及其水煎液中Cu、Mn、Zn、Fe、Se的测定和浸出率研究

用原子吸收法对黄芪及其水煎液中的Cu、Mn、Zn、Fe进行了测定 ,用紫外分光光度法测定了其中的Se ,从而得出各元素的浸出率。结果表明五种元素的浸出率为 :Cu >Zn >Mn >Se >Fe。     

Ultra high performance liquid chromatography with tandem mass spectrometry method for the determination of tetrandrine and fangchinoline in rat plasma after oral administration of Fangji Huangqi Tang and Stephania tetrandra S. Moore extracts

A rapid, sensitive, and reliable analytical method based on ultra high performance liquid chromatography with tandem mass spectrometry has been developed for the simultaneous determination of fangchinoline and tetrandrine in rat plasma. Plasma samples were pretreated by protein precipitation with acetonitrile. The analysis was performed on a C₁₈ reversed‐phase ultra high performance liquid chromatography column (2.1 mm × 100 mm, 3.5 μm, Agilent), and the flow rate was set at 0.4 mL/min. Under the experimental conditions, extraction recoveries from plasma were 68.1–72.8% for fangchinoline and 69.2–76.5% for tetrandrine. The plasma concentrations of tetrandrine and fangchinoline in rats at assigned time points were all successfully detected through exactly validated method. Good linearities were obtained in the range of 0.92–184 ng/mL for tetrandrine and in the range of 0.83–166 ng/mL for fangchinoline. The intra‐ and interday precisions for both analytes were within 11.1% and the accuracies were within the range of –10.7 to 11.3%. The developed method was then successfully applied to investigate the pharmacokinetic properties of these two alkaloids after oral administration of Stephania tetrandra S. Moore extracts and Fangji Huangqi Tang. The comparative results provided a meaningful basis for a better understanding of the practical value of the compatibility theory of traditional Chinese medicine in the clinic.     

二维相关红外光谱法与黄芪及其伪品刺果甘草的分析与鉴定

采用红外光谱的三级鉴定法分析鉴别了黄芪及其伪品刺果甘草。在一维红外光谱中,刺果甘草的1 737 cm-1CO伸缩振动峰,明显高于黄芪的1 737 cm-1特征峰,说明刺果甘草含有机酯类化合物的量相对高于黄芪。在高分辨的二阶导数谱中,刺果甘草有明显的1 620,1 317,782和516 cm-1的草酸钙特征峰,而黄芪没有。此外,两者都存在1 463,1 511和1 596 cm-1的芳香类化合物的特征峰,不同的是刺果甘草的1 468 cm-1峰的右侧还有一个1 453 cm-1的小肩峰。在二维相关红外光谱中,两者都存在1 070,1 095和1 140 cm-1的糖苷类化合物的自动峰,不同的是黄芪的1 140 cm-1的自动峰强度最大,但刺果甘草的1 090 cm-1自动峰强度最大。谱图的三级鉴定验证了黄芪及其伪品刺果甘草在糖苷类化合物、芳香类化合物和有机酯类化合物的相对含量上都是不一致的。该方法不仅可以快速有效地鉴别黄芪及其伪品刺果甘草,还提供了两者的有机酯类化合物以及芳香类和糖苷类化合物具有很大差别的一些有用的结构信息。因此,运用红外光谱法可以快速有效地分析和鉴定黄芪及其伪品刺果甘草。     

火焰原子吸收法测定黄芪中的锰

用硝酸-高氯酸混合酸(3 1)消化黄芪,在波长279．5nm处,利用火焰原子吸收法测定黄芪中锰的含量。线性回归方程为A=0．07857c 0．01282,相关系数r=0．9996,线性范围为1．5-4．5μg／mL,检出限为O．0378μg／mL,测定结果的相对标准偏差为1．54％,加标回收率为96．0％-106．5％。     

Screening anti‐allergic components of Astragali Radix using LAD2 cell membrane chromatography coupled online with UHPLC‐ESI‐MS/MS method

Huangqi (Astragali Radix), a traditional Chinese herb, is widely used in clinical therapy in China. In addition, an anti‐allergic effect of constituents in Huangqi has been reported in the scientific literature. In the present study, cell membrane chromatography coupled online with UHPLC‐ESI‐MS/MS method was developed to screen, analyze and identify the anti‐allergic components of Huangqi. The Laboratory of Allergic Disease 2 (LAD2) cell was used to establish cell membrane chromatography, which was combined with UHPLC‐ESI‐MS/MS. The coupled system was then used to screen anti‐allergic components from Huangqi. Effects of active components were verified by histamine release assay. A component retained on the LAD2 cell membrane chromatography was identified as formononetin. Bioactivity of formononetin was investigated by histamine release assay in LAD2 cells, and it was found that formononetin could inhibit histamine release in a dose‐dependent manner from 1 to 100 μm . The LAD2 cell membrane chromatography online with UHPLC‐ESI‐MS/MS method is an effective technique for screening the anti‐allergic components of Huangqi.     

红外三级鉴定法快速鉴别栽培与半野生黄芪

采用红外光谱的三级鉴定法分析鉴别了栽培黄芪和半野生黄芪。所获得的一维红外光谱、二阶导数谱和二维红外相关谱,能逐步提高红外谱图的分辨率,并从不同的角度上体现了两者的差异性。结果显示,黄芪的红外光谱主要由有机酯类化合物、醌类化合物及糖苷类物质的振动吸收带组成。两类黄芪样品的一维红外光谱和一阶导数谱整体上十分相似,只是在多糖吸收区域(1160—925cm-1)略有差异,对比该区域的二维相关红外光谱,差异主要表现在1100—1000cm-1和1150—1050cm-12个吸收带。结果表明,红外三级鉴定法可以对栽培黄芪和半野生黄芪进行快速、无损、简便的分析与鉴定。     

火焰原子吸收光谱法测定黄芪、甘草、广藿香中的铜

用硝酸-高氯酸混合酸(4 1)消解黄芪、甘草、广藿香,在波长324.7nm处,用火焰原子吸收光谱法测定黄芪、甘草、广藿香中铜的含量.线性回归方程为A=0.1861C 0.0007,相关系数r=0.9998,线性范围为0-7μg/mL,检出限为0.0032μg/mL,测定结果的相对标准偏差为0.061%,加标回收率为98.7%-103.0%.     

Rapid quantitative analysis of 18 chemical constituents in HuangQi JianZhong Tang based on UHPLC–MS

A rapid, highly sensitive, and specific analytical method using ultra-high-performance liquid chromatography-triple quadruple MS was developed to quantitatively measure 18 chemical constituents in Huangqi Jianzhong Tang (HQJZ), a famous traditional Chinese medicine formula. Chromatographic separation was performed on a Waters ACQUITY UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm) with a gradient mobile phase (A: 0.1% aqueous formic acid and B: acetonitrile) at a flow rate of 0.25 mL/min. The chromatographic peaks of 18 components were identified by comparing with the reference compounds. Multiple reaction monitoring was employed for quantitative analysis of the components. Seven batches of HQJZ samples were analyzed with a good linear regression relationship (R², .9978–.9993), precisions [relative standard deviation (RSD), 0.90%–3.60%], repeatability (RSD, 2.50%–4.00%), stability (RSD, 1.00%–4.00%), and recovery (96.10%–104.30%). Based on this established method, the present study offered a highly sensitive, specific, and rapid determination method for identification of 18 compounds, which greatly promoted the systemic quality control of HQJZ.