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。     

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.     

Development and validation of a hydrophilic interaction ultra‐high‐performance liquid chromatography with triple quadrupole MS/MS for the absolute and relative quantification of amino acids in Sophora alopecuroides L.†

Amino acids are naturally occurring compounds in many edible or medicinal plants, which possess a variety of pharmacological effects on humans. The aim of this study is to develop and validate a hydrophilic interaction LC coupled with MS/MS method for the absolute and relative quantification of amino acids without derivatization. The application of this method has been proven through 20 naturally occurring amino acids in 21 samples from different parts and phenological growth stage of Sophora alopecuroides. The method was performed on an ultra‐high performance LC separation system coupled with ESI‐MS on a triple quadrupole mass spectrometer. The proposed absolute quantitative method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery. The analysis results showed that S. alopecuroides is rich in free amino acids. In addition, relative quantitative determination of amino acids with several amino acids selected for the best accuracy was investigated. The accuracies of relative quantitative method for amino acids determinations suggest that it is feasible to quantify amino acids by the proposed relative quantitative determination method, which contributes to breaking through the choke point of lack of standards.     

苦豆子种子多糖与黄原胶的协效性研究

对苦豆子(SophoraalopecuroidesL )种子多糖(苦豆子胶)与黄原胶的协效性进行了研究.结果表明,不同配比的苦豆子胶与黄原胶混合后,其协效性不同,其中苦豆子胶与黄原胶的重量比为7∶3时,二者的协效性最高,混合液的粘度为黄原胶单溶液粘度的2倍左右,混合溶液为非牛顿流体,具有良好的触变性.研究结论是:苦豆子胶可作为黄原胶的复配胶应用于食品等工业领域.     

产酶苦豆子内生细菌筛选及其活性菌株鉴定

对苦豆子健康植株和种子内的内生细菌进行分离,共分离获得41株内生细菌.对41株菌株进行了分泌胞外淀粉酶、蛋白酶、纤维素酶、几丁质酶和β-1,3-葡聚糖酶特性的研究.结果表明,有80.5%的菌株具有蛋白酶活性;有78.0%和61.0%的菌株具有淀粉酶和纤维素酶活性;具有几丁质酶和葡聚糖酶活性的菌株则较少.经16SrRNA基因序列分析鉴定,6株高活性产酶菌株与枯草芽孢杆菌属(Bacillus subtilis)、韩国丛毛假单胞菌(Pseudomonas koreensis)、固氮阴沟肠细菌(Enterobacter cloacae)、苍白杆菌(Ochrobactrum tritici)和嗜麦芽窄食单胞菌(Stenotrophomonas maltophilia)亲缘关系较近,核苷酸序列一致性在98%以上.     

槐花中黄酮类物质提取研究

利用青海当地槐花资源，采用两种不同的方法对槐花中的黄酮类化合物进行了提取研究。比较不同提取方法的提取率及提取物中黄酮类化合物的百分含量，找出最佳提取方法。为西部开发、青海经济发展提供一条新的途径。     

多叶越南槐脂溶性成分研究

采用索氏提取法提取多叶越南槐(Sophora tonkinensis Gagnep.var.polyphylla S.Z.Huang et Z.C.Zhou)的脂溶性成分,甲酯化后,用气相色谱-质谱联用(GC-MS)进行分析,计算机检索结合人工解析进行成分分析和鉴定,共分离得到41个峰,鉴定了其中32种成分.多叶越南槐...     

秦岭苦参中苦参碱立体异构体晶体结构研究

从秦岭地区苦参中经过溶剂提取和酸化分离得到一种生物碱盐酸盐结晶1，该 晶体不对称单元含有一对新的苦参碱非对映异构体，绝对构型分别是1S，5S6S， 7R，11R，16S和1S，5S，6S，7R，11R，16R，命名为顺式新苦参碱(cis- neomatrine)和反式新苦参碱(trans-neomatrine)。1的晶体结构(C_(15)H_(24) N_2O·C_(15)H_(24)N_2O·2HCl·5H_2O)属正交晶系，空间群P2_12_12_1, a = 0. 8053(2) nm, b = 1.3464(5) nm, c = 3.0971(9) nm, V = 3.3580(18)nm~3, Z = 4, μ=0.244 mm~(-1), F(000) = 1432, R = 0.0467, wR = 0.1129。顺式新苦参 碱和反式新苦参碱的A环、B环和C环为式构象，D环为半椅式构象，其中A／B为反式 稠合，A／C和B／C为顺式稠合，两种立异构体的区别是顺式新苦参碱的C／D顺式稠 合，反式新苦参碱的C／D反式稠合。     

黄酮化合物的偶氮显色反应及其应用研究

在pH 10 4的NH4Cl NH3 ·H2 O缓冲溶液中 ,对磺基氯化重氮苯可与芦丁 ,桑色素 ,染料木甙 ,槲皮素 ,橙皮甙 ,黄岑甙和大豆甙等 7种黄酮化合物发生偶氮显色反应 ,反应产物的最大吸收波长 ,除黄岑甙为 380nm外 ,其余均在 4 30nm ,显色反应的灵敏度依上述顺序逐渐减弱。其中芦丁的摩尔吸收光系数最大 ,为 3 2 8× 10 4L·mol-1·cm-1,大豆甙摩尔吸光系数最小 ,为 8 30× 10 2 L·mol-1·cm-1。提出的分光光度分析方法 ,用于槐米和豆粕中黄酮化合物的测定 ,RSD为 0 2 5 %～ 4 4 8% ,回收率在 99 3%～ 10 5 0 %之间     

大球蚧天敌的研究

呼和浩特市行道树国槐上的蚧虫主要种类为枣球蜡蚧(Eulecanium gigantea)和槐花球蚧(E.kuwanai)，通过研究其天敌有两种，分别为球蚧蓝绿跳小蜂(Blastothrix sericae)和北京举肢蛾(Beijing utila)．对这两种天敌的形态特征、生活史、生活习性及与蚧虫的关系进行了研究．