超声辅助提取山桃仁中苦杏仁苷的工艺优化

为优化桃仁中苦杏仁苷超声波辅助提取工艺,采用单因素研究乙醇体积分数、提取温度、提取时间、液料比和超声工作时间、超声处理温度6个因素对苦杏仁苷得率的影响,在此基础上应用正交试验对提取工艺进行优化,并用HPLC法对桃仁中苦杏仁苷的含量进行测定。结果表明,最佳工艺为乙醇体积分数85%、提取温度85℃、提取时间60 min、料液比1∶35(g∶mL)、超声处理时间30 min、超声处理温度70℃,同时此条件下苦杏仁苷的得率为2.88%。     

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%.     

高效液相色谱法定量分析甲氨基阿维菌素苯甲酸盐

研究用HPLC定量分析甲维盐的方法。色谱条件如下:150mm×4.6mm不锈钢柱,用Hypersil,C185μm粒径,孔径300A;流动相:甲醇+水=80+20;流速1.0mL/min;紫外检测器波长254nm。本方法在1～8μg进样范围内和峰高呈线性。相关系数值(r)为0.9997。甲维盐分析方法的回收率为99.42%。     

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。     

10％多·三环悬浮种衣剂的高效液相色谱分析

本文叙述的是采用反相高效液相色谱法即以甲醇+水+氨水为流动相,C8柱和紫外检测器同柱分离测定多菌灵和三环唑,结果表明三环唑和多菌灵的标准偏差分别为0.19和0.087,变异系数分别为0.87%和0.54%,平均回收率分别为99.6%和100.8%,线性关系分别为0.9994和0.9992。