邻苯二甲醛-尿素柱前衍生高效液相色谱法快速检测枸杞中牛磺酸

干枸杞经粉碎、匀浆、离心后,通过阳离子交换柱脱去样品中其它氨基酸,再通过Ｚｏｒｂａｘ－Ｃ８柱进行柱前衍生分离。衍生剂：Ａ．４％ＯＰＡ甲醇溶液;Ｂ．尿素∶磷酸钠盐缓冲液（ｐＨ６．８）＝１∶３（Ｗ／Ｖ）。流动相：甲醇∶０．０１ｍｏｌ／Ｌ乙酸钠溶液（ｐＨ６．８）＝３５∶６５（Ｖ／Ｖ）。紫外检测波长３３０ｎｍ。牛磺酸浓度在０．１～１．０ｍｍｏｌ／Ｌ范围内可被定量测定。回收率可达１００．３１％±１．９８％,变异系数（ＣＶ）为１．９４％。     

苯甲酰化展青霉素和青霉酸的高效液相色谱紫外吸收测定法

建立了一种快速、灵敏检测痕量展青霉素（ｐａｔｕｌｉｎ）和青霉酸（ｐｅｎｉｃｉｌｌｉｃａｃｉｄ）的新方法。对酞内酰胺苯甲酰氯（４（２－ｐｈｔｈａｌｉｎｕｄｙｌ）ｂｅｎｚｏｙｌｃｈｌｏｒｉｄｅ,简称ＰＩＢ－Ｃｌ］为柱前衍生试剂同展青霉素和青霉酸衍生反应,衍生物用ＯＤＳ柱分离,乙腈－水（４７：５３,Ｖ／Ｖ）作流动相,紫外检测器检测（λ＝３００ｎｍ）。以２倍信噪比计算最低检出限,展青霉素２．０ｐｍｏｌ,青霉酸１０ｐｍｏｌ。     

高效液相色谱-电化学检测法同时测定人血浆中的组织胺和去甲肾上腺素

报道了用高效液相色谱配合电化学检测器同时分析组织胺（Ｈｉｓｔ）和去甲肾上腺素（ＮＡ）的方法。用邻苯二甲醛（ＯＰＡ）进行柱前衍生,流动相为Ｖ（乙酸钠缓冲溶液）Ｖ（乙腈）＝７３,检测器电位＋０．７Ｖ,线性范围为０．０１５～５μｇ／Ｌ（ｒ＝０．９９８）,平均回收率为９５％。方法灵敏、准确,重复性好,分析速度快,可用于临床检测。     

氢化物－气相色谱的元素光度检测器

研究开发的一种新型的元素光度检测器主要用于锗、砷、锡和锑的氢化物气相色谱检测，具有高灵敏，高选择性。它是在普通火焰光度检测器的基础上加装了特制的滤光片改制而成的。对锗、砷、锡和锑的检测限分别为３．０×１０￣（－１１）ｇ、７．０×１０￣（－１１）ｇ、７．０×１０￣（－１０）ｇ和１．１×１０￣（－８）ｇ，相对标准偏差分别为１．８％、２．４％、２．６％和３．０％。     

未衍生高效液相色谱法测定螺旋藻粉中γ-亚麻酸含量

建立了未衍生高效液相色谱法测定螺旋藻粉中γ－亚麻酸（ＧＬＡ）的方法。采用Ｃ８反相柱,以乙腈：四氢呋喃：水（含０．４％乙酸）＝６２：３：３５（Ｖ／Ｖ／Ｖ）为流动相,示差折光检测器检测,测定了同一批螺旋藻粉中ＧＬＡ含量为１．３９％,标准偏差０．０４３２,变异系数３．１１％,回收率为９３．９０％￣９８．９３％,本方法快速,重现性及准确度均令人满意。     

氢化物－气相色谱的元素光度检测器

 研究开发的一种新型的元素光度检测器主要用于锗、砷、锡和锑的氢化物气相色谱检测，具有高灵敏，高选择性。它是在普通火焰光度检测器的基础上加装了特制的滤光片改制而成的。对锗、砷、锡和锑的检测限分别为３．０×１０￣（－１１）ｇ、７．０×１０￣（－１１）ｇ、７．０×１０￣（－１０）ｇ和１．１×１０￣（－８）ｇ，相对标准偏差分别为１．８％、２．４％、２．６％和３．０％。     

脱乙酰壳多糖化学修饰电极测定铂的研究

用脱乙酰壳多糖修饰电极为工作电极，阳极溶出伏安法测定痕量铂。在ｐＨ＝２￣３的ＫＣｌ－ＨＣｌ底液中，－０．３Ｖ富集２ｍｉｎ，静止１５ｓ，以０．２Ｖ／ｓ扫速阳极溶出，峰电位在－０．１６Ｖ（ｖｓ．ＳＣＥ），铂（Ⅳ）离子浓度在０．５￣５．０μｇ／ｍＬ范围内与峰高呈线性关系。富集１０ｍｉｎ后，可检测０．０２５μｇ／ｍＬ铂（Ⅳ）。该法用于贵金属矿样的测定，无需分离，结果满意。用循环伏安法、紫外光谱和拉曼光谱研     

高效液相色谱法快速测定猪肉中醋酸地塞米松残留物

本文研究了一种快速、简便测定猪肉中醋酸地塞米松残留的高效液相色谱法。肉样用二氯甲烷提取，甲醇溶解残留物，２４０ｎｍ处紫外检测。在０．０６￣１．５０μｇ／ｋｇ浓度范围内，醋酸地塞米松线性相关系数为０．９９９２，相对标准偏差分别为２．９２％（日内）和４．７８％（日间）。空白肉样添加０．０５￣０．２０ｍｇ／ｋｇ醋酸地塞米松，其回收率在７５．６０％￣８７．９０％。本法可检测出样品中低至５０μｇ／ｋｇ的醋酸     

HPLC检测柑桔类水果中无机溴化合物残留量

采用ＨＰＬＣＳｈｉｍ－ｐａｃｋＩＣ－Ａ１柱，紫外检测器测定柑桔类水果中无机溴残留量，样品经氢氧化钠乙醇溶液水解，灰化后进行ＨＰＬＣ分析。方法简便，重复性好（ＣＶ＝０．９５～８．６１％），样品检出限为１０￣（－６），添加回收大于９０％。     

高效液相色谱法检测弹性蛋白中锁链素

用高效液相色谱技术对弹性蛋白水解液中锁链素进行了测定。单一锁链素,锁链素、酪氨酸、苯丙氨酸混合液及弹性蛋白水解液经Ｃ１８柱分离,甲醇－水（２８,Ｖ／Ｖ）洗脱,紫外检测器２８０ｎｍ检测。锁链素与酪氨酸峰面积比（ＣＡ）和峰高比（ＣＨ）分别为１．４％和３．４％,标准曲线浓度范围０．１６～０．６４ｍｇ／Ｌ时相关系数为０．９９５６。结果表明：上述色谱条件可定量测定弹性蛋白中锁链素含量,无需将锁链素与水解液中其它氨基酸加以分离,而仅需同其它２７５ｎｍ有吸收的组分区分。     

Studies on the behaviour of α-, β- and γ-cyclodextrins and some derivatives under reversed-phase liquid Chromatographic conditions

The separation processes of α-, β- and γ-cyclodextrins and their various methyl derivatives have been investigated with Knauer polarimetric (Chiralyser) and refractive index (RI) detectors. RP18 and RP8 hydrocarbon packings and an NH₂ bonded phase were applied as stationary phases. Aqueous methanolic or ethanolic solutions were used as mobile phases. It has been found that the Chiralyser detector response is approximately linear at low concentrations of solutes and that its detection capabilities are about 40 times better than those of the RI detector. Differences in the order of elution of α-, β- and γ-cyclodextrins have been observed for various stationary phases as well as for various mobile phase compositions. The optimal conditions for analytical determinations of cyclodextrins and their derivatives have been discussed.     

二元复杂共混体系组成的SEC-LS分析

提供了一种利用体积排阻色谱-光散射(SEC-LS)联用技术来解决二元复杂共混体系组成的定量分析问题.基于体积排除色谱的绝对定量化原则,首先从理论上分析了共混物的光散射响应因子与组成呈线性关系.通过分析六组复杂共混体系的光散射响应因子与组成的关系,验证了该线性关系确实存在.进而利用该线性关系计算了共混体系的组成.在某些共混体系中,通过光散射响应因子得出的组成比利用示差法得出的组成更加接近原料组成.通过分析这两种方法产生误差的来源,阐述了产生该现象的原因.     

Aqueous sec analysis of cationic polymers as gene carriers

Cationic polymers have been receiving much attention as non-viral gene vectors.The aqueous mobile phase was optimized in combination with Shodex OHpak SB columns for size-exclusion chromatography(SEC)analysis of disulfide-containing poly(ethylene imine)(PEI)derivatives used in gene delivery.Addition of acetonitrile in mobile phase was shown to be able to suppress the hydrophobic interactions between polymer analytes and the stationary phase.The absolute molecular weights and distributions of the cationic polymers were determined directly from online SEC-MALS(multi-angle light scattering)/RI(refractive index detector).The results demonstrate that a good SEC separation of disulfide-containing PEI derivatives used in gene delivery with little band broadening was achieved.     

Determination of sugar alcohols in confectioneries by high-performance liquid chromatography after nitrobenzoylation

A method was developed for the determination of sugar alcohols, meso-erythritol, xylitol, D-glucitol, D-mannitol, maltitol and parachinit by high-performance liquid chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride. HPLC was performed on a phenyl column, using acetonitrile-water (67:33) as mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10-250 microg/ml range. The average recoveries of the sugar alcohols from four sugarless confectioneries spiked at 5 and 10% levels of six sugar alcohol standards ranged from 73.2 to 109.0% with relative standard deviations ranging from 0.7 to 9.0%. The detection limit of the developed method was 0.1% for the above sugar alcohols contained in the samples.     

Electrochemical synthesis of glycoconjugates of 3β-hydroxy-Δ-steroids by using non-activated sugars and steroidal thioethers

A new protocol for the electrochemical synthesis of glycoconjugates is presented. Thioether derivatives of cholesterol and other sterols were subjected to anodic oxidation in the presence of a sugar alcohol affording glycoconjugates with the sugar linked to a steroid moiety by an ether bond. The isomeric 6β-3α,5α-cyclo-steroidal thioethers proved to be better sterol donors than the normal 3β-Δ⁵-steroidal thioethers.     

Determination of alcohols by high-performance liquid chromatography with fluorimetric detection after pre-column derivatisation with carbazole-9-N-acetic acid and chromatographic behaviour of alcoholic derivatives

Alcohols were derivatised to their carbazole-9-N-acetic acid (CRA) esters with 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC.HCl) as the dehydrating agent. Studies on derivatisation conditions indicated that the coupling reaction proceeded rapidly and smoothly in the presence of a base catalyst in acetonitrile to give the corresponding sensitively fluorescent derivatives. The retention behaviour of alcohol derivatives was investigated by varying mobile phase compositions (ACN-water and MeOH-water). The parameters from the equation log k'=A-BX were evaluated by retention data of derivatives using an isocratic elution with different mobile phases. The results indicated that the parameters derived allowed computation of retention factors in good agreement with experiments. At the same time, a general equation was derived that makes possible predictions of partition coefficient in binary mobile phases with different proportions of organic solvent to water based on some simple regression analysis. The LC separation for the derivatised alcohols containing higher carbon alcohols showed good reproducibility on a reversed-phase C18 column with gradient elution. The detection limits (excitation at 335 nm, emission at 360 nm) for derivatised alcohols (signal-to-noise ratio=3:1) were in the range of 0.1-0.4 pg per injection.     

高效液相色谱法测定克鲁维酵母菊芋发酵液中的乙醇,糖和有机酸类代谢成分

建立了高效液相色谱法同时分析菊芋发酵液中的乙醇和有机酸的方法.采用HPLC有机酸分析柱, 流动相为0.01 mol/L H2SO4,流速为0.5 mL/min, 以紫外和示差折光检测器作为双通道检测手段,同时对克鲁维酵母菊芋发酵液中的柠檬酸、α-酮戊二酸、葡萄糖、丙酮酸、果糖、琥珀酸、乳酸、甘油、乙酸、乙醇进行了定量分析,本方法的回收率为95.8%～109.6%;RSD为0.33%～4.0%,结果表明,本方法简单、快速、准确,适用于监控克鲁维酵母发酵产物并指导整个发酵过程条件的优化.     

The High Performance Liquid Chromatography and Detection of Phospholipids and Triglycerides. III. Response of the Differential Refractive Index and Ultraviolet Absorption Detector

Abstract

A liquid chromatographic differential refractive index detector (RI) and an ultraviolet absorption (at 195 nm) detector (UV) were studied for detection of triglyceride (TG) and phospholipid (PL) molecular species. It was found that the log UV/RI detector response ratio was linearly related to the log of the number of conjugated double bonds (degree of unsaturation) of the lipid in a predictable fashion, indicating the usefulness of the combination of both detectors in TG and PL analysis. The detection limit of the RI detector for TG and PL was found to be 5 × 10 ^?7 M or as sensitive as the UV detector for saturated TG and PL.     

C_(60)Cl_n对阴离子活性聚苯乙烯和对活性聚苯乙烯-b-聚异戊二烯的偶联作用

富勒烯(Fullerene)独特的结构和性质吸引了高分子界的广泛的关注．迄今，已通过和自由基共聚、活性自由基聚合、阳离子聚合、阴离子聚合、以及配位聚合等诸多方法相结合制备出了种类繁多的富勒烯高分子衍生物，不仅如此，富勒烯家族的重要分支——富勒烯卤化物，其独特的分子结构和具有的新性质也引起了人们的重视．     

β-砜基醇衍生物还原中的基团效应

比较芳香族砜基和脂肪族砜基对钠-汞齐还原β-砜基醇衍生物反应的影响。在还原β-苯基砜基醇衍生物的反应条件下,β-叔丁基砜基醇衍生物并不能得到还原去砜基的烯烃。β-苯基砜基醇衍生物可能是经过单电子转移消除的机理,而β-叔丁基砜基醇甲磺酰化物则经α-砜基碳负离子的消除过程得到烯烃基砜。