毛细管胶束电动色谱法分离测定胆红素亚组分

用毛细管胶束电动色谱法成功地分离和定量测定了血清及胆汁中α，β，γ及δ等４种胆红素亚组分。二牛磺酸胆红素浓度在５１０μｍｏｌ／Ｌ以下时，峰面积与浓度呈良好的线性关系，二牛磺酸胆红素浓度即使为１．５μｍｏｌ／Ｌ时仍可检测出明显的定量峰。用一份２５５μｍｏｌ／Ｌ的二牛磺酸胆红素标准液进行重复性检测，第１次定量结果为２６０μｍｏｌ／Ｌ，出峰时间１６ｍｉｎ；第５０次电泳结果为２３８μｍｏｌ／Ｌ，出峰时间１６．７ｍｉｎ。     

碳纤维汞膜微电极1.5次微分伏安法测定米托蒽醌的研究

米托蒽醌（ＭＸＴ）能吸附在碳纤维汞膜微电极表面，阴极溶出时，产生一个灵敏的１．５次微分溶出峰，其峰电流和米托葱酿的浓度在１．０×１０－５ｍｏｌ／Ｌ～１．３×１０－９ｍｏｌ／Ｌ范围内具有良好的线性关系，经３ｍｉｎ的富集，检出限可达１．０×１０－１０ｍｏｌ／Ｌ，据此建立了测定ＭＸＴ的灵敏的新方法，本文讨论了实验条件，并对血样中的ＭＸＴ进行了测定。     

胆绿素的溶出伏安法研究及胆红素的间接测定

本对胆绿素的吸附溶出分析法进行了研究，发现胆绿素在Ｎａ２ＨＰＯ４－Ｎａ３ＰＯ４（０．１ｍｏｌ／Ｌ，ｐＨ１１．５）缓冲溶液中可在－０．８３Ｖ（ｖｓ，ＳＣＥ）左右产生灵敏的吸附溶出峰，该峰可检测出低至５×１０＾－９ｍｏｌ／Ｌ胆绿素。在通常条件下，通过０．５ｍｉｎ预富集后溶出，可使峰高提高约一个数量级。应用此法间接测定了小牛血清中的胆红素含量。     

金在脱乙酰壳多糖学修饰电极上的电化学行为及分析应用

用脱乙酰壳多糖化学修饰电极为工作电极，阳极溶出伏安法测定痕量金。在ｐＨ１￣２的ＫＣｌ－ＨＣｌ底液中，超始电位０．２０Ｖ，终止电位１．３０Ｖ，富集时间５ｍｉｎ，以－０．１／ｓ扫速阳极溶出，峰电位在１．００Ｖ（ｖｓ．ＳＣＥ），Ａｕ（Ⅲ）浓度在０．１０ｍｇ／Ｌ￣１０ｍｇ／Ｌ范围内与峰高呈线性关系。在富集１０ｍｉｎ时，可检测０．２５ｍｉｇ／ＬＡｕ，大大提高了测定灵敏度，用于矿样测定，无需分离，结果满意。用     

一阶导数差示脉冲极谱法用于甲硝唑的定量研究

本实验运用一阶导数差示脉冲极谱法对甲硝唑及其制剂进行了定量研究。在０．００１ｍｏｌ／Ｌ氯化钾－０．００１ｍｏｌ／Ｌ盐酸－水（１＋０．２＋４８）的底液中，甲硝唑于－０．８００Ｖ（ｖｓ Ａｇ／ＡｇＣｌ）处出现一良好的一阶导数差示脉冲极谱峰，在５０～３００μｇ／ｍＬ范围内，药物浓度与其导数峰幅值呈线关系，检测限为８．０×１０＾－８ｍｏｌ／Ｌ。本法操作简便，快速，灵敏，结果准确。     

穿心莲内酯的电化学研究

用单扫描示波极谱法在０．０５ｍｏｌ／ＬＮＨ４ＣＬ＋０．２５ｍｏｌ／ＬＮＨ３．Ｈ２Ｏ中，穿心链内酯有一灵敏的还原峰，２５℃时，峰电位为－１．６０Ｖ（ｖｓ．ＳＣＥ），峰电流与浓度在０．０１～１．２ｍｇ／Ｌ和１．４～２６ｍｇ／Ｌ范围内有良好的线性关系，检测限为６ｎｇ／ｍＬ。用本法测定天然中药穿心链中总内酯的含量，其结果令人满意。实验证明穿心链内酯的电极过程为可逆的逐级电子过程，Ｈ２Ｏ２可催化该还原峰，另     

丙酸睾丸素的吸附阴极溶出伏安法研究

在ｐＨ为６．０的Ｂ－Ｒ缓冲溶液中，丙酸睾丸素于电位－１．４Ｖ（ｖｓ．ＳＣＥ）左右处出现一个灵敏的附阴溶出峰。经５ｍｉｎ富集后，阴极溶出峰电流与浓度在１．３８×１０＾－＾８－７．３×１０＾－＾８ｍｏｌ／Ｌ范围内成线笥关系，该方法用于注射液中丙酸睾丸素含量测定，回收率８０％－８６％。检测下限为４．１×１０＾－＾９ｍｏｌ／Ｌ。     

金在脱乙酰壳多糖化学修饰电极上的电化学行为及分析应用

用脱乙酰壳多糖化学修饰电极为工作电极，阳极溶出伏安法测定痕量金。在ｐＨ１～２的ＫＣｌ－ＨＣｌ底液中，起始电位０．２０Ｖ，终止电位１．３０Ｖ，富集时间５ｍｉｎ，以０．１Ｖ／ｓ扫速阳极溶出，峰电位在１．００Ｖ（ｖｓ．ＳＣＥ），Ａｕ（Ⅲ）浓度在０．１０ｍｇ／Ｌ～１０ｍｇ／Ｌ范围内与峰高呈线性关系。在富集１０ｍｉｎ时，可检测０．０２５ｍｇ／ＬＡｕ，大大提高了测定灵敏度，用于矿样测定，无需分离，结果满意。用紫外光谱和拉曼光谱研究了该法的电极过程机理。     

金橙G螯合形成树脂分离富集地质样品中的微量贵金属

主要研究了金橙Ｇ螯合形成树脂分离富集地质样品中金、铂、钯的最佳实验条件。在柱高大于１６ｃｍ，０．１ｍｏｌ／Ｌ ＨＣｌ介质的样品溶液以小于或等于０．５ｍＬ／ｍｉｎ流速过柱，用０．１ｍｏｌ／Ｌ ＨＣｌ的３％硫脲溶液以小于或等于０．５ｍＬ／ｍｉｎ流速洗脱金、铂、钯（和铑），都能同时定量富集。用火焰原子吸收光谱法测定，回收率均在９５％￣１１０％之间。经地质样品加标准回收实验，结果令人满意。证明这种以磺酸基     

铁的单点络合滴定法研究

本研究了Ｆｅ＾３＋的单点络合滴定法，导出了定量关系式，比较了以铂电极为指示电极和以ＰＶＣ膜四氯络铁（Ⅲ）阴离子电极为指示电极时电位测量的稳定性及所得的分析结果。在Ｆｅ＾３＋浓度为１．０００×１０＾－３ｍｏｌ／Ｌ时，１８次实验的平均值为１．０２×１０＾－４ｍｏｌ／Ｌ，相对偏差小于１．７％；Ｆｅ＾３＋在５．０×１０＾３ｍｏｌ／Ｌ以上时，相对偏差小于０．１％；其浓度小于１０＾－３ｍｏｌ／Ｌ而大于５×１     

高效液相-荧光检测法快速测定血清中的色氨酸

 利用色氨酸具有自然荧光的特点 ,建立了测定血清中色氨酸浓度的高效液相 荧光检测分析方法。血清标本经高氯酸沉淀蛋白后取上清液进行分析 ,柱为Nova PakC18柱 ,流动相为 5mmol/L磷酸二氢钾水溶液 ,流速为 1mL/min ,激发波长为 2 5 4nm ,荧光检测波长为 338nm。该法检测色氨酸浓度的线性范围为 0 4 9μmol/L～ 4 90 0 0 μmol/L ,最低检测限为 0 10 μmol/L ,回收率为 97 2 %～ 98 6 % (平均值为 97 9% ) ,批内、批间相对标准偏差均小于 5 % ,苯丙氨酸、酪氨酸、5 羟色胺和 5 羟吲哚乙酸等物质对该法均无干扰。     

高效液相色谱法快速测定人血清中丙戊酸含量

建立了血清中丙戊酸的高效液相色谱快速分析法。用ＺｏｒｂａｘＯＤＳ柱,ｐＨ４．２硫酸水溶液为流动相,检测波长２１０ｎｍ,流速０．８ｍＬ／ｍｉｎ,线性范围０．８２μｍｏｌ／Ｌ～１．８ｍｍｏｌ／Ｌ（ｒ＝０．９９６）,最低检测限０．８２μｍｏｌ／Ｌ,平均回收率为９８．３２％±２．２７％,日内与日间的变异系数分别为３．３１％（ｎ＝５）和４．８２％（ｎ＝７）。     

Protective effects of various Chinese traditional medicines against experimental cholestasis

In a previous paper, we reported that methanol extracts obtained from 13 Chinese traditional medicines showed remarkable choleretic effects in normal rats. This paper examines the protective effects against experimental cholestasis induced by carbon tetrachloride (CCl4) or alpha-naphthylisothiocyanate (ANIT) in rats. No medicines, including sodium dehydrocholate and 1-phenylpropanol which are used clinically as choleretic drugs, inhibited the decrease of bile flow induced by CCl4. On the other hand, Intinko-to, Saiko-seikan-to and Bohu-tusyo-san revealed marked improvement of the dysfunction in bile secretion induced by ANIT. These three medicines inhibited the decrease of excretion of bile acid or bilirubin in the bile. They also exerted a protective effect against the alterations of serum components induced by ANIT, i.e., of glutamic oxaloacetic transaminase, glutamic pyruvic transaminase, alkaline phosphatase and the concentration of serum bilirubin. These results indicate that methanol extracts of Intinko-to, Saiko-seikan-to and Bohu-tusyo-san demonstrate not only choleretic effects but also improvement of cholestasis and liver parenchymal injury in rats.     

HPLC同时检测血清和尿样中肌酐、假尿苷、尿酸

用反相高效液相色谱法同时测定了３９例糖尿病患者的血清和尿样中的假尿嘧啶核苷、肌酐和尿酸,并与２４ｈ尿白蛋白排泄量进行了比较分析。发现血清假尿嘧啶核苷是糖尿病肾病早期诊断的一种新颖而敏感的指标,有助于连续监测肾脏的功能状态以了解病程的转归。     

高效液相色谱法测定大鼠神经组织中的硝酸盐和亚硝酸盐

 建立了大鼠神经组织中亚硝酸盐和硝酸盐的高效液相色谱测定方法,以用于研究一氧化氮在糖尿病慢性神经病变中的作用。在1 μmol/L～25 μmol/L的浓度范围内,NO2-和NO3-的峰面积与浓度的线性相关系数>0.991;最低检测浓度分别为0.2 μmol/L和0.5 μmol/L;日内、日间相对标准偏差<14%。对各实验组大鼠的初步测定结果表明,糖尿病组及糖尿病胰岛素(IGF)治疗组的NO2-和NO3-水平均低于对照组。 关键词：高效液相色谱法;一氧化氮;硝酸盐;亚硝酸盐;糖尿病神经病变     

Novel method for high-performance liquid chromatography of azo derivatives of conjugated and unconjugated bilirubin

A method for the separation and quantitation of ethyl anthranilate or p-iodoaniline azo derivatives of bile pigments was developed using reversed-phase high-performance liquid chromatography. A convenient separation was achieved in 15 min, permitting the quantitation of the unconjugated azo-dipyrrole (alpha o) and its glucuronide (delta), xyloside (alpha 2) and glucoside (alpha 3) conjugates. The pathological beta- and gamma-azo pigments, derived from bilirubin glucuronide isomers that occur in cholestatic bile or plasma, are also detected in this system. The results of this method as applied to bile from 25 healthy dogs were in excellent agreement with the values obtained by reversed-phase chromatography of bilirubin and its mono- and dimethyl esters produced from the corresponding conjugates by alkaline methanolysis. This system permits the sensitive and convenient determination of bilirubin and its conjugation pattern in biological fluids.     

Rapid determination of lysine in biological samples by isocratic liquid chromatography.

A simple, rapid, and sensitive method was developed for detection and quantitation of lysine (Lys) in various biological samples by isocratic liquid chromatography (LC). Samples containing Lys and other amino acids were derivatized with 9-fluorenylmethyl chloroformate (FMOC-CI). The mobile phase used for isocratic elution was 50 mmol/L sodium acetate buffer (pH 4.20)-acetonitrile (43 + 57, v/v). Lys was detected with a UV detector at 265 nm. The derivatized Lys eluted from a LiChrospher 100 RP-18 (150 x 4.0 mm id) column at a retention time of 5.6 min. The limit of detection was 0.73 mumol/L (signal-to-noise [S/N] ratio, 3:1), and the limit of quantitation was 2.37 mumol/L (S/N ratio, 10:1). Lys recoveries from fortified biological samples were > 97.5%. Average Lys contents found in rumen fluid samples collected before the morning feeding and at 2.0, 4.0, and 6.0 h after feeding were 4.26, 3.34, 3.58, and 3.82 mumol/L, respectively. The hydrolysate of a sample of mixed rumen microorganisms collected before the morning feeding was determined to contain 1.372 mumol/mg microbial nitrogen in the form of Lys. The Lys concentrations of human plasma, goat plasma, human urine, and goat urine were 140.0, 102.0, 58.0, and 32.0 mumol/L, respectively.     

新的匀相清除法测定血清高密度脂蛋白胆固醇

为建立利用混合表面活性剂做为抑制剂测定血清高密度脂蛋白胆固醇的新匀相法,将血清标本中的LDL-C、VLDL-C、CM等脂蛋白组分用HLB值为13.2的混合表面活性剂特异性清除,仅剩余HDL-C裂解参加胆固醇反应。结果表明,该法的线性区间为3.90 mmol/L;回收率为96.2%～103.7%;批内变异系数(CV)和批间变异系数(CV)分别为0.65%～2.88%、1.25%～3.56%;该法与参考方法回归方程及相关系数分别为y=1.010 2 x+0.078 8,r=0.976 2,相关性良好;当c(LDL-C)<12.8 mmol/L、c(TG)<12 mmol/L、ρ(胆红素)<320 mg/L、ρ(血红蛋白)<14 g/L对该法测定不干扰。该法实现了用表面活性剂为清除剂的HDL-C匀相法直接测定,在测定过程中既无明显浊度产生,也不堵塞自动分析仪的管道,而且具有良好的精密度和准确性,适合临床上推广应用。     

Effect of Tridax procumbens (Linn.) on bile duct ligation-induced liver fibrosis in rats

The present study was undertaken to clarify whether methanolic extract of Tridax procumbens prevents liver fibrosis in rat. The hepatic fibrosis was induced by 28 days of bile duct ligation in rats. The 4-week treatment with Tridex procumbens reduced the serum aspartate aminotransferase (U?L?1), glutamate pyruvate transaminase (U?L?1), alkaline phosphatase (IU?L?1), lactate dehydrogenase (IU?L?1), total bilirubin (mg?dL?1), direct bilirubin (mg?dL?1) and hydroxyproline (mg?gm?1) content in liver and improved the histological appearance of liver section. The results of this study led us to conclude that T. procumbens can reduce the degree of hepatocellular damage and may become antifibrotic agent for liver fibrosis.     

Measurement of bilirubin partition coefficients in bile salt micelle/aqueous buffer solutions by micellar electrokinetic chromatography

The partition coefficients for the distribution of bilirubin between aqueous phosphateborate buffer and cholic, taurocholic, taurodeoxycholic, and taurochenodeoxycholic micelles have been measured by micellar electrokinetic chromatography at pH 8.5. Determination of the partition coefficients required that the critical micelle concentration and partial specific volumes be determined for each bile salt. Critical micelle concentrations were slightly higher for the trihydroxy bile salts. Partial specific volumes of the bile salt micelles differed very little from each other, and for each bile salt they were constant over the concentration range studied, which was typically from slightly above the critical micelle concentration to 35 mM. Capacity factors were corrected for the effects of applied voltage by extrapolation of the capacity factor to zero applied volts. The free solution mobility of bilirubin, determined in the absence of bile salt, was also corrected for the effects of applied voltage. Plots of extrapolated capacity factor versus phase ratio yield the partition coefficient as the slope of a linear fit to the data. Partition coefficients for bilirubin were significantly higher for dihydroxy bile salts than for trihydroxy bile salts.