高效液相色谱测定小蔓长春花中长春胺的方法优化

采用不同比例的甲醇-1%二乙胺(pH 7.5)、甲醇-1%碳酸铵、乙腈-1%二乙胺(pH 7.5)、乙腈-1%碳酸铵为流动相,在比对保留时间的基础上加以光谱确认,并对小蔓长春花提取液中长春胺保留时间及其分离情况进行研究,以选择测定长春胺的最佳流动相体系.结果显示:在甲醇-碳酸铵、乙腈-碳酸铵、乙腈-二乙胺体系中,长春胺峰很难完全分离,其光谱扫描结果与标准品不一致;而在甲醇-二乙胺体积比为65∶35时,长春胺峰可实现基线分离,其光谱扫描结果与标准品一致,且长春胺在0.05~0.5 g/L范围内与峰面积线性关系良好(R2=0.997),平均加样回收率为100.71%(n=5),RSD=2.23%.研究表明,甲醇-1%二乙胺(体积比为65∶35,pH 7.5)为测定小蔓长春花中长春胺含量的最佳流动相体系,可用于小蔓长春花药材的质量监控.     

生姜辛辣部位的高效液相色谱(HPLC)指纹图谱研究

采用HPLC法分析了4个居群生姜丙酮回流-乙醚萃取物中的多酚类化合物,建立了有较好专属性的HPLC指纹图谱,比较了姜辣素含量及其得率。     

高效液相色谱法分离测定香兰素

用６０％乙醇提取香荚兰豆的香兰素,经高效液相色谱法分离,在紫外波长３３０ｍｍ处测定,选取适当的流动相,能快速,准确地测定出香兰素,最低检测含量可达到０．０１μｇ．     

反相高效液相色谱测定番茄组织中的水杨酸

DetendnationofSalicylicAcidinTOmatObyReve~Phaseaam--PerforrmceliqUidChro~twyXUYOu-Ping,MAZhi~Chao(~~,~~~dy,~310029)CAJXin-Zhong(~ofAn~,~~-d~ity,~310029)水杨酸是一种酚类物质,广泛存在于自然界。它与植物的开花、气孔关闭、种子发芽、产热、膜通透性以及离子吸收等许多生理生化过程有关[1]。有人认为水杨酸是一种新的植物激素[2],最近几年研究结果认为它与植物抗病性也有关系,是植物的系统性诱导抗病性（systemacqui。dr。sta。e,SAN）信号传递系统中的重要组成部分［’j。番茄组织中水杨酸含量的高效液相色谱…     

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     

高效液相色谱测定车间空气中的甲醛

将盛有 DNPH 液的气泡吸收瓶,吸收车间空气中甲醛.2,4-二硝基苯肼和醛定量反应形成二硝基苯腙.Shimadu ODS(φ4.6×150mm)柱上分离,紫外检测器(360nm)测定.以保留时间定性、峰面积定量.本法线性回归方程相关系数大于0.999,变异系数0.48%,最低检出浓度为0.17mg/m~3.     

高效液相色谱法测定比卡鲁胺片的含量

目的:建立高效液相色谱法测定比卡鲁胺片含量和含量均匀度的方法。方法:采用SHIMADZUCLC-ODS(150mm×6.0mm,5μ)色谱柱,以0.1%磷酸二氢钾溶液-乙腈(50:50)为流动相,272nm波长处检测。结果:比卡鲁胺在0.05mg·ml-1～0.20mg.ml-1浓度范围内线性关系良好(r=0.9995),平均回收率为99.5%,RSD=0.9%(n=9)。结论:本方法简便、准确度好、精确度高。     

检测植物组织中多胺含量的高效液相色谱法

对反相高效液相色谱技术测定苯甲酰化多胺的方法进行了探讨 ,确定和研究了苯甲酰化反应的最佳温度、时间和影响苯甲酰化多胺稳定性的因素 ,优化了多胺的色谱分析条件     

Rapid analysis of naphthalene and its metabolites in biological systems: Determination by high-performance liquid chromatography/fluorescence detection and by plasma desorption/chemical ionizations mass spectometry

A rapid procedure for the determination of naphthalene and its metabolites in bile of rainbow trout and mice is described. The integrated analytical techniques combine high-performance liquid chromatography/ultraviolet fluorescence detection and plasma desotption/chemical ionization mass spectrometry for identification and quantitation. After separation by reverse-phase liquid chromatography, naphthalene and its metablolites are detected and quantitated by ultraviolet fluoresence spectometry. Identification of two metabolites is confirmed by mass spectometry. A direct insertion probe tip for a conventional chemical ionization mass spectometer was modified to obtain spectra of thermally labile compounds. A spectrum of less than 100 ng of naphthyl glucuronide, a labile glucuronic acid conjugate of 1-naphthol, was obtained with this system.     

Assay of galactosyltransferase by high-performance liquid chromatography

Galactosyltransferase catalyzes transfer of galactose from UDP-galactose to glucose or N-acetylglucosamine with resultant formation of galactosides and UDP. In this new assay galactosyltransferase activity is measured by determining UDP by isocratic high-performance liquid chromatography on an amino-bonded column monitored spectrophotometrically. Concurrently, unreacted UDP-galactose and breakdown products arising from UDP-galactose (UMP and uridine) are also determined. The new technique does not require radioactive substrates, permits usage of saturating concentrations of UDP-galactose, and provides monitoring of side reactions.     

Superior resolution of gamma-crystallins from microdissected eye lens by cation-exchange high-performance liquid chromatography

A novel procedure is presented for the rapid quantitative analysis of eye lens gamma-crystallins and beta s-crystallin by ion-exchange high-performance liquid chromatography on Synchropak CM300. At least six different gamma-crystallin gene products can be resolved from the soluble fraction of calf lens extract. This method is applicable to the analysis of microsections from individual lenses, and can be used to rapidly characterize spatial variations in gamma-crystallin composition which occur with aging and cataractogenesis.     

高压液相荧光检测法检测血浆同型半胱氨酸

目的:建立高压液相荧光检测法测定血浆中同型半胱氨酸(homocysteine,Hcy)的方法.方法:应用Symmetry ShieldTMRP18色谱柱,0.08 mol/L醋酸钠1%甲醇为流动相,与巯基特异结合的荧光物质SBD-F衍生巯基来检测血浆中的同型半胱氨酸浓度.结果:该法的平均回收率为95.8～100.8%,相对标准差为1.2～2.0%.结论:本检测法方法准确,可用于实验室样品的测定.     

多重PCR-DHPLC快速检测食品中产志贺毒素大肠杆菌

应用多重PCR(motiplex PCR)结合变性高效液相色谱技术(denaturing high-performanceliquid chromatography,DHPLC)建立了快速检测食品中产志贺毒素大肠杆菌O111和O157的方法.以基因wzxO111、rfbEO157为靶基因,建立多重PCR-DHPLC方法,进行特异性和灵敏度测试,同时进行RT-PCR检测比较灵敏度.该方法具有良好特异性,可以一次PCR扩增同时检测O111、O157;灵敏度达到25 CFU/mL.129份牛肉样品中检出1例O111,3例O157阳性;74份鸡肉样品中检测出O111、O157阳性各1例,67份蔬菜样品中未检测到O111、O157.本文建立O111、O157多重PCR-DHPLC检测方法,操作简便,特异性强,适用于产志贺毒素大肠杆菌筛选检测.     

Determination of proton dissociation constants by ion-exchange high-performance liquid chromatography

The common methods to determine dissociation constants of solutes, e.g., uv spectrophotometry, potentiometry, and conductimetry, are accurate but require at least 1 nmol of compound. High-performance liquid chromatography (HPLC) allows 1 pmol of a uv-absorbing compound to be detected. By adjusting the polarity of the mobile phase, reverse and normalphase properties of an ion-exchanger can be minimized, resulting in a high correlation between charge and retardation of the solute. Thus, the degree of ionization of several compounds was monitored in mobile-phase compositions of different pH values using cation exchange. The pK values of several pterin derivatives corresponded to those obtained by other methods. In addition, pK values of two unidentified pterin derivatives were determined, using only 20 pmol of each.     

Analysis of polyamines in higher plants by high performance liquid chromatography

A sensitive (0.01-1 nmol) method has been developed for the analysis of polyamines in higher plant extracts based on high performance liquid chromatography (HPLC) of their benzoyl derivatives (Redmond, Tseng 1979 J Chromatogr 170: 479-481). Putrescine, cadaverine, agmatine, spermidine, spermine, and the less common polyamines nor-spermidine and homospermidine can be completely resolved by reverse phase HPLC, isocratic elution with methanol:water (64%, v/v) through a 5-μm C₁₈ column, and detection at 254 nm. The method can be directly applied to crude plant extracts, and it is not subject to interference by carbohydrates and phenolics. A good quantitative correlation was found between HPLC analysis of benzoylpolyamines and thin layer chromatography of their dansyl derivatives. With the HPLC method, polyamine titers have been reproducibly estimated for various organs of amaranth, Lemna, oat, pea, Pharbitis, and potato. The analyses correlate well with results of thin layer chromatography determinations.     

A rapid high-performance liquid chromatographic procedure for the simultaneous determination of methionine, ethionine, S-adenosylmethionine, S-adenosylethionine, and the natural polyamines in rat tissues

A method for the analysis of S-adenosyl-L-methionine (SAM) and S-adenosyl-L-ethionine (SAE) and their major metabolites by high-performance liquid chromatography is described. The procedure allows the simultaneous analysis of the natural polyamines, putrescine, spermidine, and spermine, and some of the major amino acids, methionine, tyrosine, and tryptophan. The uv absorbance at 254 nm is used for the determination of the SAM and SAE analogs, whereas the polyamines and amino acids are analyzed by fluorescence detection after postcolumn derivatization with o-phthalaldehyde. The method allows SAM and polyamine determinations by direct injection of the tissue extracts without prepurification. The procedure is applied to study the effects of DL-ethionine treatment on the SAM, SAE, methionine, and polyamine levels in various tissues of rats.     

Simple method for the simultaneous isolation and determination of fumonisin B1 and its metabolite aminopentol-1 in swine liver by liquid chromatography--fluorescence detection

An analytical method based on high-performance liquid chromatography (HPLC) combined with fluorescence detection (FL) has been developed for the simultaneous determination of fumonisin B1 (FB1) and its totally hydrolized metabolite aminopentol-1 (AP1) in pig liver. The sample preparation is based on a single solid phase extraction (SPE). o-Phthalaldehyde (OPA) was used for pre-column derivatization before the programmed reversed-phase analysis on phenylhexyl column. The developed method shows good repeatibility for inter- and intra-day precision as well as adequate linearity of calibration curves (r2 was 0.9855 for FB1 and 0.9831 for AP1). Average recoveries from the matrix were 93.6% for FB1 and 95.3% for AP1. The limit of quantification (LOQ) in swine liver was 75 microg/kg for FB1 and 42 microg/kg for AP1.