高效液相色谱-光电二极管检测器法测定栀子中乌索酸的研究

建立反相高效液相色谱法测定了栀子中乌索酸的质量分数,同时采用光电二极管阵列检测器检测乌索酸色谱峰的纯度。色谱柱为Nuc leosil C18柱(4.6 mm×250 mm,5μm),流动相为甲醇-水(85∶15,V/V),流速0.8 mL.m in-1,检测波长205 nm,柱温25℃。乌索酸在0.1696~1.5264μg范围内线性关系良好(r=0.9999),检出限为0.3 mL-1(3σ),平均回收率为98.0%。方法简便,准确,重现性好,线性范围宽,适于测定栀子药材中乌索酸的质量分数。     

高效液相色谱法测定血浆中同型半胱氨酸

建立了一种高效液相色谱-库仑阵列电化学测定血浆中同型半胱氨酸的方法。采用3-2-羧乙基膦作为还原剂还原巯基间形成的二硫键,用0.1 mol.L-1HC lO4来沉淀血浆蛋白,离心取上清,进样分析。在0.40~50.00μmol.L-1范围内,线性关系良好。加标平均回收率是98.43%,RSD%是4.35%。该方法简单、快速、灵敏。     

梯度洗脱高效液相色谱法测定桑叶中3种活性成分的含量

建立同时测定桑叶中绿原酸、芦丁和槲皮素含量的分析方法。色谱柱为NUCLEODUR C18 RP(250 mm×4.6 mm,5μm),光电二极管检测器,流动相为甲醇-质量分数0.5%磷酸水溶液,梯度洗脱程序为0 min(30:70)-15min(30:70)-25min(50:50)-35min(85:15)-40min(30:70);流速0.8 ml.min-1,检测波长为350 nm。绿原酸、芦丁和槲皮素的线性范围分别为0.1144~1.0296μg(r=0.9996)、0.0436~0.3924μg(r=0.9999)和0.0452~0.4068μg(r=0.9997),平均回收率分别为97.7%(RSD=1.7%)、98.4%(RSD=2.2%)和100.6%(RSD=1.5%)。方法快速简便,专属性强,重复性好,可作为桑叶中绿原酸、芦丁和槲皮素的定量分析方法。     

高效液相色谱测定蕨类植物中氨基酸含量

以5种蕨类植物(大羽贯众、美丽复叶耳蕨、黄山鳞毛蕨、狗脊蕨和紫萁)根状茎为研究材料,利用邻苯二甲醛柱前衍生高效液相色谱法分析了材料中的氨基酸成分.鉴于材料中蛋白质含量较低,测定方法中增加了样品的使用量并采用了梯度洗脱程序.结果表明,测试的5种蕨类植物所含总氨基酸含量较低,很少有超过5%,尤其在狗脊蕨中只有1.74%.在...     

高效液相色谱-柱后光化学衍生法测定变性淀粉中黄曲霉毒素含量的研究

本文采用高效液相色谱-柱后衍生法对变性淀粉中的黄曲霉毒素G2、G1、B2和B1含量进行测定.样品采用乙腈-水(84:16,v/v)提取,经免疫亲和柱净化,C18色谱柱分离,以乙腈-甲醇-水(10:30:60,v/v)为流动相进行洗脱,用HPLC光化学衍生-荧光检测器检测样品含量.结果表明,4种黄曲霉毒素的标准曲线线性均...     

高效液相色谱法测定黄瓜皮中绿原酸含量

目的:建立高效液相色谱法测定黄瓜皮中绿原酸含量的方法.方法:采用Zorbax Eclipse XDB-C18色谱柱(150 ×4.6 nm,5 μm);流动相:甲醇- 0.4%磷酸溶液(25∶75);流速:1.0 ml·min-1;检测波长:326nm;柱温:30℃.结果:绿原酸的线性范围为0.0111～0.1332 ...     

高效液相色谱法测定浓缩苹果汁中棒曲霉素

建立了高效液相色谱法 (HPLC)测定浓缩苹果汁中棒曲霉素含量的方法。用乙酸乙酯提取浓缩苹果汁中棒曲霉素 ,碳酸钠水溶液净化提取液 ,蒸干乙酸乙酯层 ,其残留物用醋酸缓冲液溶解。棒曲霉素的含量测定采用HypersilODS (5 μm ,2 5 0mm×4 6mmi d)色谱柱 ,流动相V(乙腈 ) :V(醋酸盐缓冲液 ) :V(水 ) =5 :3:2 ,流速 1ml min ,检测波长 2 76nm。结果表明 :棒曲霉素浓度与峰面积有很好的线性关系 ;用HPLC测定浓缩苹果汁中棒曲霉素的含量可操作性强、准确度高 ,棒曲霉素回收率高达 99 2 %,重现性好 (RSD为 0 4 %) ;灵敏度高最小检出量为 10 μg L。     

植物组织中赤霉酸含量的高效液相色谱测定

赤霉素(GAs)是最难检测的一类植物激素。目前,测定GAs最有效的手段是气-质联用色谱(GC-MS),但并非所有实验室都能具备。免疫学方法已经用于GAs含量测定,国内已建立了GA_4-RIA(~3H),但GA_4的抗血清还存在对GA_1,GA_3,GA_7的交叉     

高效液相色谱法直接测定当归中阿魏酸的含量

建立了一种高效液相色谱法直接测定当归中阿魏酸的含量。色谱柱为Shim-pack CLC-ODS(6.0 mm i.d×150 mm,5μm),流动相为甲醇—1.0%冰醋酸水溶液(体积比为25∶75),流速为1.0 mL/min,检测波长为313 nm。研究结果表明:阿魏酸的线性范围为1.0~10.0 mg/L,回归方程为A=13.352 8C 0.013 6(r=0.998 5),最小检测限为10 ng,加样平均回收率为94.67%,相对标准偏差(RSD)为1.57%。方法操作简便、快速、灵敏、准确。     

Specific Proline and Hydroxyproline Detection Method by Post-column Derivatization for High-performance Liquid Chromatography

A specific detection method for hydroxyproline by post-column derivatization with 7-chloro-4-nitrobenzo-2-oxa-l,3-diazole was developed after chiral resolution by ligand-exchange chromatography. The addition of ethylenediaminetetraacetic acid to the reaction mixture was effective to achieve the post-column reaction. The calibration curve for trans-4-hydroxy-L-proline shows linearity from 7.6 pmol up to 7600 pmol.     

离子交换高效液相层析法测定腺苷酸环化酶活性

用离子交换高效液相层析（ＨＰＬＣ）分离并同步测定脑组织腺苷酸环化酶（ＡＣ）反应生成的ｃＡＭＰ,从而直接测定ＡＣ活性。１００℃加热１ｍｉｎ终止ＡＣ反应后,混合物在０℃放置２ｈ。在此期间,反应体系中残留的ＡＴＰ水解酶将反应混合物中大部分剩余的ＡＴＰ水解除去。用二氯甲烷抽提除去罂粟碱等干扰物质,使混合物中的ｃＡＭＰ同蓁物质在Ｓｈｉｍ－Ｐａｋ ＷＡＸ－１阴离子交换ＨＰＬＣ术上基线分离,并可定量测定,用此方     

High-performance Liquid Chromatography of Aflatoxins with Fluorescence Detection

Aflatoxins B_l, B₂, G₁ and G₂ were quantitatively detected by high-performance liquid chromatography on a 12 µl flow-cell in the fluorometric detector using the mobile phase of toluene system instead of chloroform, dichloromethane or methanol system. Various kinds of columns and mobile phases were tested, and fine mutual separation of all the four aflatoxins without quenching their fluorescence was achieved by using sHica gel column and toluene- ethyl acetate-formic acid-methanol (89.0: 7.5: 2.0: 1.5 v/v/v/v). The relationship between the fluorescence peak area and the amount injected was linear in the range of 0.3 ng to 120 ng. This method, as applied to food and feed extracts, is sensitive at the 10~20 ppb levels of the four kinds of aflatoxins.     

Separation and Quantification of Abscisic Acid and its Metabolites by High-performance Liquid Chromatography

A technique for the separation and quantitative estimation ofabscisic acid and its metabolic products, phaseic acid and dihydrophaseicacid by high performance liquid chromatography (HPLC) is described.The efficiency of two HPLC columns, LiChrosorb RP-18 and LiChrosorbNH₂ is compared. The method has been tested using extracts fromtomato plants and some of the results are presented. Abscisic acid, dihydrophaseic acid, phaseic acid, chromatography, tomato, Lycopersicon esculentum, Mill     

A Simplified Method for the Quantitative Determination of Indoleacetic Acid by High Performance Liquid Chromatography with a Fluorometric Detector

Quantitative analysis of endogenous IAA contents of radish plantextracts by high performance liquid chromatography with a fluorometricdetector was refined by using a C-18 SEP-PAK cartridge for thepurification procedure and indolepropionic acid as the internalstandard. The C-18 SEP-PAK cartridge efficiently purified theIAA from the acidic ether-soluble fraction of the plant extractswhen the pH of the fraction injected into the cartridge waskept under 3.5. Both of the recovery rates for IAA and indolepropionicacid were over 90% for the extraction and purification procedure.The endogenous IAA content in green radish seedlings, correctedby internal standard methods with indolepropionic acid, was20.2 ng/g fr wt. This was in good agreement with the value correctedwith radiolabeled ¹⁴C-IAA, 20.8 ng/g fr wt. (Received May 18, 1983; Accepted August 31, 1983)     

Fundamental Procedures for Determining Ergosterol Content of Decaying Plant Material by Liquid Chromatography

Portions of published procedures for measurement of ergosterol content of decomposing plants were examined for their influence upon ergosterol yield. Common methods of treatment of plant samples prior to sterol extraction (e.g., oven drying, freezing, lyophilization) led to reduced recoveries of ergosterol (ca. 20 to 80%). The least destructive method was direct placement and storage in methanol. Photoconversion of ergosterol is not likely to cause losses during analysis, but losses are likely if there is insufficient mixing during neutral-lipid partitioning from base-hydrolysis reagents. Homogenization (two times for 2 min) and refluxing (2 h) in methanol were equally effective in extracting ergosterol. Direct extraction in base-hydrolysis reagents was less effective (by ca. 40%).     

高效液相色谱法测定毛豆中吡虫啉残留量

采用高效液相色谱法测定毛豆中吡虫啉农药残留。试样用二氯甲烷超声波提取,中性氧化铝柱净化,石油醚去除脂类杂质,以0.2%冰乙酸水溶液-乙腈(70:30,体积比)为流动相,配备Agilent TC-c18柱、高效液相色谱紫外检测器检测(HPLC-UV),外标法定量。实验表明,毛豆样品中吡虫啉添加回收率为84.0%~102.8%,相对标准偏差(n=6)为6.8%~10.9%,样品中吡虫啉最低检测浓度为0.003 mg/kg。     

Determination of Chlorophenols in Soils by a Method Involving Alkaline Extraction and Solid-phase Preconcentration Prior to High-performance Liquid Chromatography

A well-reproducible method for determining five common chlorophenols in soils is described. Chlorophenols were extracted from a soil with sodium hydroxide and, after being acidified to pH 6.5, the extract was cleaned by partitioning between chloroform and sodium hydroxide. After adjusting the pH value to 5.5, the sample was concentrated in a C-18 minicolumn. The chlorophenols were desorbed with methanol, the extract was basified, the solvent volume was reduced to 100 μl, and the concentrated extract was acidified. An aliquot was analyzed by HPLC with UV detection (225 nm). Recovery experiments were performed at concentration levels of 1 ppm, 0.1 ppm, and 0.01 ppm. Recovery levels between 65% and 83% with a standard deviation of ±3.75 were achieved at the concentration level of 0.1 ppm. Detection limits between 2 ppb (2,4,6-trichlorophenol) and 2.5 ppb (4-chloro-3-methylphenol) were determined.