微波消解-原子吸收光谱法测定槐花和大黄中微量元素

采用微波消解-火焰原子吸收光谱法和石墨炉原子吸收光谱法测定了中药槐花和大黄中铜、铁、锌、镉、铬和铅。研究了槐花和大黄的微波消解试剂和消解条件。在原子吸收光谱测定的最佳条件下测定槐花和大黄中铜、铁、锌、镉、铬和铅。方法的回收率在89．2％～112．0％之间。     

正交实验法优选苦参总碱提取工艺

目的：在单因素实验的基础上采用L9（3^4）正交试验优选苦参总碱提取工艺．方法：以浸膏得率、苦参总碱提取率为评价指标,选择乙醇浓度、加乙醇量（倍）、提取时间（h）为考察因素,利用L9（3^4）正交试验法优选乙醇提取苦参总碱的最佳工艺．结果：最佳提取工艺条件为用75％乙醇8倍量,提取lh.结论：该提取工艺方法方便而结果可靠．     

西藏不同区域砂生槐在不同采收时间的花、茎、叶及种子中苦参碱、氧化苦参碱含量比较

目的：测定西藏不同区域产砂生槐在不同采收时间花、茎、叶及种子中的苦参碱与氧化苦参碱的含量,为其合理采收利用提供科学依据。方法：使用高效液相色谱（HPLC）：SHIMADZUC18色谱柱（150X4．6）;流动相：甲醇（0．05mol／L）-磷酸二氢钠溶液（含磷酸2ml／L）一高氯酸钠（15ml：85ml：O．5g）,检测波长为215rim,流速为0．7ml／min,柱温为室温。结果：种子中氧化苦参碱、苦参碱含量较高,最高的为日喀则七月份采种子,苦参碱含量（24．48mg／g）,氧化苦参碱含量（51．125mg／g）。结论：砂生槐花、茎、叶及种子中均合有苦参碱和氧化苦参碱,不同区域、不同采收时间其含量有差异,种子采收7月份最佳,利用叶子应在6-7月。     

苦参的染色体研究

对苦参（Ｓｏｐｈｒａ ｆｌａｖｅｓｃｅｎｓ Ａｉｔ）。进行了核型分析，结果表明：染色体数目为２ｎ＝１８，核型公式为Ｋ（２）＝１８＝１０ｍ＋８ｓｍ，核型属“２Ａ”型。核型不对称系数为５９．４２％，染色体的相对长度组成为２ｎ＝１８＝６Ｍ２＋１２Ｍ１。     

山豆根总黄酮不同提取方法的比较

分别采用常规回流提取法、超声提取法、微波辅助萃取法及索氏提取法对中药山豆根进行提取;以芦丁为对照品,采用分光光度法测定提取物中总黄酮的含量;以总黄酮的含量为考察指标,优选出最佳提取方法.结果表明,4种提取方法中,常规回流提取法总黄酮含量最高,微波辅助萃取法和超声提取法总黄酮含量较高,索氏提取法总黄酮含量最低;综合考虑,...     

微波辅助提取-高效液相色谱法测定苦参中5种苦参生物碱的含量

取粒径在0.18～0.25mm的药材粉末于提取罐中,用水作提取剂,在110℃、压力为15MPa、功率为780W的条件下进行微波提取(PMAE)5min,经离心后取上清液为提取液。提取液经无水乙醇处理提纯后得到待测物的甲醇溶液,从中分取部分溶液按选定条件用液相色谱-质谱(LC-MS)联用做定性分析,用高效液相色谱(HPLC)做定量分析。LC-MS结果表明:提取液中含有氧化苦参碱、氧化槐果碱、槐定碱、苦参碱和槐果碱,与其它3种提取方法比较,PMAE的提取率高且提取时间短。HPLC定量时,采用C18色谱柱,以不同比例的甲醇、乙腈和0.1%氨水溶液(pH 10.3)的混合溶液作流动相进行梯度淋洗,可分离上述5种生物碱,以峰面积和浓度间的线性关系进行定量。5种生物碱的回收率在93.9%～101.0%之间,测定值的相对标准偏差(n=5)在0.53%～2.6%之间。     

Simultaneous determination of phytochemicals and low-weight organic acids in Sophora japonica bud and premium noni juice through column-switching liquid chromatography connected with ion chromatography system

In this work, a liquid chromatography connected with an ion chromatography by the column-switching technique was developed for the simultaneous determination of three phytochemicals (scopoletin, rutin, and quercetin), three anions (chloride, sulfate, and phosphoric), and seven organic acids (lactic, acetic, propionic, formic, malic, oxalic, and citric acid) in Chinese traditional herbs, S. japonica bud and premium noni juice. A concentration column was used to collect organic acids and anions, and then the concentrated analytes were eluted to an analytical column by column-switching technique in which target analytes could be separated successfully and detected simultaneously within 70?min. This method showed good linearity with the linear correlation coefficients in the range of 0.9971–1.0000. The relative standard deviations of the peak areas were all less than 5.63% (n?=?6). The limits of detection (LOD, S/N?=?3) of anions and organic acids were in the range of 0.0006–0.0857?mg/L, whereas phytochemicals were in the range of 0.0123–0.0197?mg/L. Recoveries were in the range of 86.53–117.01% for the spiked sample. This method was successfully applied to the determination of the low-weight organic acids and phytochemicals in Chinese traditional herbal medicines, S. japonica bud and premium noni juice.     

Determination of quinolizidine alkaloids in Sophora flavescens and its preparation using capillary electrophoresis

A simple and accurate capillary electrophoresis method was developed for the determination of four quinolizidine alkaloids in Sophora flavescens and Kuhuang injection. Optimum separation of the analytes was obtained on a 65 cm x 75 microm i.d. uncoated fused-silica capillary using a aqueous buffer system of 60 mmol L(-1) sodium borate at pH 8.5, with applied voltage and capillary temperature of 12 kV and 25 degrees C, respectively. Detection wavelength was set at 204 nm and jatrorrhizine was used as the internal standard. Good linear relationships between peak-area ratios and concentrations of the analytes were observed over the concentration range 0.044-0.792 mg mL(-1) for matrine, 0.142-1.926 mg mL(-1) for oxymatrine, 0.0377-0.3393 mg mL(-1) for sophocarpine and 0.0664-1.062 mg mL(-1) for sophoridine. The recoveries of four alkaloids ranged between 93.08 and 101.4% with relative standard deviations from 0.7 to 9.2% (n = 6) as determined by standard addition. The limits of detection for four alkaloids were determined to be over the range 8.8-48.0 microg mL(-1). Contents of four alkaloids in Sophora flavescens and three alkaloids in Kuhuang injection were successfully determined under the optimum conditions.     

On the absolute configuration of matrine: Crystal structure of matrin-1-IUM-trichlorozincate

The title compound crystallizes in the monoclinic space group P2₁ with a = 7.804(1)?, b = 13.597(2) ? c = 9.093(1) ?, β= 108.41(1)°, V = 915.5(2)?³, Z = 4, R = 0.0231, wR2 = 0.0475 (Siemens P4 diffractometer with MoK _α radiation, 3994 reflections collected at room temperature, 204 parameters refined). It is a zwitterionic complex (having Zn-O coordination bond of 2.003(2) ?) with a positive charge on the N1 atom of matrine molecule and a negative charge on the ZnCl₃ group. In the matrine molecule, N16 and H11 atoms are located on the opposite sides of the plane defined by C11, C15, C17 atoms and deviate from the plane by 0.075(3) ? and 0.839(3) ?, respectively, indicating a trans C-D ring junction. Therefore, the compound can be named trans-matrine. The D ring of matrinium demonstrates a distorted sofa conformation, while the other rings adopt chair forms. The A-B, A-C, B-C and C-D ring pairs have trans, cis, cis and trans junctions, respectively. The absolute configuration of the matrine molecule is 1S, 5S, 6S, 7S, 11R, 16R. Original Russian Text Copyright ? 2009 by Z. M. Jin, L. L. Ma, W. X. Wei, and Y. Q. Li The text was submitted by the authors in English. Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 197–200, January–February, 2009.     

Determination and Comparison of Phytoestrogens in Both Crude and Parched Flos Sophorae Immaturus by Capillary Electrophoresis with Electrochemical Detection

A method using high-performance capillary electrophoresis with electrochemical detection (CE-ED) has been developed for content comparison of phytoestrogens in both crude and parched Flos sophorae immaturus. Genistin, genistein, rutin, kaempferol and quercetin are important active constituents in this plant. The effects of several factors, such as acidity and concentration of running buffer, separation voltage, applied potential and injection time, were investigated to find the optimum conditions. Detection limits (S/N=3) ranged from 1.1 × 10^–7 to 2.8 × 10^–7gmL^–1 for all five analytes. This method was successfully used to analyse both crude and parched Flos sophorae immaturus after a relatively simple extraction procedure, and the assay results were satisfactory.