超微粉碎对黄连解毒汤中栀子苷和小檗碱溶出的影响

目的:比较普通粉碎和超微粉碎对黄连解毒汤中栀子苷和小檗碱溶出量的影响.方法:用HPLC法测定.结果:超微粉碎可增加栀子苷和小檗碱的溶出量,在超声提取下超微细粉中栀子苷和小檗碱含量分别比细粉提高26.26%和37.07%.结论:超微粉碎没有改变黄连解毒汤固有的药效学物质,但对黄连解毒汤中栀子苷和小檗碱溶出量而言,超微粉碎有重大意义.     

Unsaturated vitamin b(12) binding capacity in human and ruminant blood serum - a comparison of techniques including a new technique by high performance liquid chromatography

A new technique by High Performance Liquid Chromatography (HPLC-gel permeation) shows promise as a tool to separate and quantitate the Unsaturated Vitamin B(12) Binding Capacity (UBSC) of the individual Vitamin B(12) binders in blood serum. This method, although not as rapid as protein-coated charcoal or cellulose separation techniques, is more applicable for use with large numbers of samples than gel filtration. The use of a radioactivity detector to monitor the eluant from the column permitted automation of the method. Comparable results for UBBC and for the UBBC of individual binders were obtained when samples were analyzed by gel filtration and HPLC. The HPLC method proved suitably precise and the recovery of added cyanocobalamin was acceptable. It is proposed that HPLC be the method of choice for measurement of the USBC of binders of Vitamin B(12) in blood serum.     

Enantioselective degradation kinetics of metalaxyl in rabbits

Metalaxyl [methyl-N-(2′-methoxyacetyl)-N-(2,6-dimethylphenyl)-d,l- alaninate] is a potent phenylamide fungicide. The (−)-(R)-isomer accounts for most of the fungicidal activity. A possible stereo and/or enantioselective kinetics of metalaxyl in rabbits was investigated by intravenous injection. The concentrations of (−)-(R)- and (+)-(S)-metalaxyl in plasma, liver, and kidney tissue were determined by HPLC with a cellulose-Tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase and gas chromatography-mass spectroscopy. After intravenous administration of racemic metalaxyl (40 mg/kg), the (+)-(S)-enantiomer levels in plasma, liver, and kidney decreased more rapidly than the (−)-(R)-isomer. The area ratio of the (−)-(R)-/(+)-(S)-enantiomer under the concentration-time curve (AUC_0 → ∞) in plasma after drug application was 1.62. The total plasma clearance value of the (+)-(S)-enantiomer was 1.53 and higher than that of the (−)-(R)-enantiomer. The [R]/[S] ratio in plasma was >1 for standard rac-metalaxyl at each time point. The other pharmacokinetic parameters of the enantiomers were also different. The results indicate substantial stereoselectivity in the degradation of metalaxyl enantiomers in rabbits.     

西瓜中类胡萝卜素的高效液相色谱法分析

通过高效液相色谱法对西瓜中的类胡萝卜素进行分析,采用Vydac201TP54C18色谱柱,比较2种不同流动相的检测结果,表明乙腈:甲醇:二氯甲烷=75:20:5(V:V:V)的分离效果较好;初步定性分析确定西瓜中含有7种以上类胡萝卜素。     

HPLC法检测发酵玉米粉中的黄曲霉毒素B1、B2、G1、G2

发酵玉米粉用甲醇∶水(80∶20,V∶V)提取黄曲霉毒素(AFT),经免疫亲合柱(IAC)分离纯化、在线光化学衍生器柱后衍生化后,反相高效液相色谱(HPLC)荧光检测器测定AFT(B1、B2、G1、G2)含量。4种毒素在0.5ng/g和2ng/g2个水平下,样品加标回收率平均值分别为B188.0%和93.6%、B285.2%和85.3%、G192.4%和91.5%、G289.6%和85.6%;5次测定的标准差分别为:B12.5和6.3、B23.5和6.0、G12.8和9.0、G22.3和6.9;4种毒素的方法检出限均达到0.05ng/g。     

生乳与巴氏杀菌乳中糠氨酸含量及其测定方法研究

本试验研究了生乳与巴氏杀菌乳中糠氨酸含量及其测定方法,并提出糠氨酸作为巴氏杀菌乳中复原乳成分的标示物质,可鉴定巴氏杀菌乳中是否掺入复原乳.研究结果表明,生乳中糠氨酸含量应低于7 mg/100 g;乳粉中糠氨酸含量大于135 mg/100 g;不含复原乳的巴氏杀菌乳中糠氨酸含量应小于12 mg/100 g.使用高效液相色谱(HPLC)紫外检测糠氨酸平均偏差＜5%(n=5);回收率为98.2%.     

苯磺隆·甲磺隆·氯磺隆混合物的液相色谱分析

本文以甲醇 水 冰乙酸为流动相，采用C18不锈钢柱，检测波长240nm，对苯磺隆、甲磺隆、氯磺隆混合物进行反相高效液相色谱定量分析。该方法的标准差别分别为0.081、0.013和0.013，变异系数为0.886%、0.268%和0.256%，回收率为99.39%、99.29%和99.28%，线性相关系数为苯磺隆r=0.9994、甲磺隆r=0.9992、氯磺隆r=0.9991，线性方程为苯磺隆y=1360088.17x 1389384、甲磺隆y=972186.69X-21262.8、氯磺隆y=789773.50X 86258.8。     

21％聪唑禾草灵·乙菝氟草醚乳油液相色谱分祈

本文采用高效液相色谱法,以C18柱为固定相,甲醇+水为流动相,用236nm紫外检测器定量测定唑禾草灵、乙羧氟草醚混剂的有效成分含量。本方法的变异系数分别为0.06%、0.40%;标准偏差分别为0.009、0.032;平均回收率分别为99.13%、100.05%;线性相关系数分别为0.9993、0.9998。     

HPLC法检测果实组织中内源IAA、ABA方法的改进

以柑橘、猕猴桃、桃和葡萄果实为材料,在前人研究的基础上,结合近10年的研究积累,针对果实组织材料富含多酚类和色素等杂质的特点,对以往的HPLC分析植物内源激素的植物材料前处理方法进行了改进,并配合适宜的HPLC色谱条件,用于果实组织内源IAA和ABA的分析测定。结果显示该改进方法适合果实组织内源IAA和ABA的分析测定。     

离子对高效液相色谱法测定复方甲硝唑片中甲硝唑和维生素B6含量

建立了同时测定复方甲硝唑片中甲硝唑和维生素B6含量的离子对HPLC方法.采用ODS色谱柱,流动相为磷酸二氢钾和庚烷磺酸钠水溶液(每1L中含磷酸二氢钾13.6 g与庚烷磺酸钠1.0 g)-甲醇-三乙胺(85∶15∶0.4),用磷酸调pH至2.8;检测波长290 nm,以峰面积计算,外标法定量.甲硝唑和维生素B6的线性范围分别为100～300 μg/mL(r=0.999 9)和5～50 μg/mL(r=0.999 9);平均回收率分别为100.2%(RSD=1.0%,n=6),99.8%(RSD=1.2%,n=6).该方法测定结果准确,操作简便,回收率高.