糖尿病人头发中微量元素Cu、Zn、Cr的极谱测定

用Cu,Zn-乙二胺-8-羟基喹啉极谱体系测定糖尿病人发中的微量元素Cu,Zn,用NH2OH·HCl-一氯乙酸-乙酸钠-5-Br-PADAP极谱体系测定糖尿病人发中Cr(Ⅲ),结果良好.糖尿病人头发中铜、铬含量高于健康人,而锌含量较健康人低.     

肿瘤患者放疗前后血清八种微量元素含量的研究

对临床、病理、放射线或CT检查确诊的82名癌肿患者，在放疗前后和对42名健康人进行了微量元素铁、锌、铜、锰、硒，铬、钴、镍的分析。研究结果显示：1．癌肿患者血清铜、镍、锰、铬、钴的含量比健康人高，而血清锌、铁、硒的含量却比健康人低；2．血清Cu／Zn、Cr／Zn、Co／Zn、Ni／Zn的比值癌肿患者均比健康人高，而Fe、Zn、Se／Zn的比值却相反。因此，可根据血清铜升高、血清锌降低，血清铜／锌比值升高的特点。用于癌肿的早期诊断；3．癌肿患者放疔后血清铁、锌含量进一步下降，铜、锰、铬的含量也出现降低，唯有硒的含量有所上升。因此，放疗时应注意补充铁、锌、铜元素。     

增感效应导数火焰原子吸收光谱测定金属铜和铜合金中的微量铬

提出了增感效应导数火焰原子吸收光谱测定金属铜和铜合金中微量铬的新方法。研究了表面活性剂十二烷基硫酸钠对铬的增感效果。导数技术与增感效应相结合的可使火焰原子吸收光谱的灵敏度提高６８倍。本法测定金属铜和铜合金中的微量铬取得了满意效果。     

流动注射-导数火焰原子吸收光谱测定植物油中的镍、锰、铬和铅

提出了流动注射－导数火焰原子吸收光谱测定植物油中微量镍、锰、铬和铅的新方法，流动注射进样技术克服了常规火焰原子吸收法耗样量大和基体干扰严重的缺点，导数技术应用于火焰原子吸收可提高方法的灵敏度和信号的选择性，流动注射与导数技术相结合应用于火焰原子吸收成功地测定了常规火焰原子吸收法和流动注射－火焰原子吸收法难以测定的植物油中微量镍、锰、铬和铅。镍、锰、铬和铅的特征浓度（μg/mL)，分别为0.0054、0.0034、0.0067、0.025，相对标准偏差在0.3%-2.8%的范围内。     

固体表面化学发光分析 Ⅲ.超基性岩和钢中铬的微量测定

本文在不渗透阻挡滤纸上，用过氧化氢将Ｃｒ（Ⅵ）还原为Ｃｒ（Ⅲ），建立了Ｌｕｍｉｎｏｌ－Ｈ２Ｏ２－Ｃｒ（Ⅲ）体系的固体表面化学发光分析法。铬测定的线性范围为１．０～１０００ｎｇ，检测限为０．１３ｎｇ。与微量离子交换柱结合，快速测定了微量超基性岩和钢铁试样中的铬。     

纯钒、钒合金及高钒钢中微量铬的测定

铬(Ⅵ)和二苯卡巴肼反应的灵敏度高,选择性较好,已普遍应用于痕量铬的比色测定。因为钒(V)与二苯卡巴肼生成黄色络合物严重干扰铬的测定,所以钒存在时测定微量铬是困难的。在“色层分离-二苯卡巴肼分光光度法测定纯铁、纯铜及钢中微量铬”的一文中,曾详细地研究了铬的色层分离等条件。本文在该工作的基础上,鉴于钒(V)在酸性介质中(pH<1)以VO_2~+离子存在的性质,进一步研究了应用阴离子交换活性氧化铝色层吸附柱(简称吸附柱)从大量的     

急性心肌梗塞患者血清硒,锌,铜,钙,镁,铁,锶含量的测定

分别对２９例急性心肌梗塞（ＡＭＩ）病人和４０例健康人进行血清中七种微量、常量元素含量测定，结果表明，ＡＭＩ患者血清Ｓｅ、Ｚｎ、Ｃａ较正常对照组明显降低；血清Ｃｕ显著增高，血清Ｆｅ、Ｍｇ较对照组低，差异不显著；血清Ｓｒ两组无差异。对ＡＭＩ患者与血清硒及各元素间相互关系进行了探讨，指出调整人体微量、常量元素的不平衡状况，对冠心病和ＡＭＩ的发生、发展和康复有一定的临床意义。     

烧伤病人血和尿中微量元素的相互关系与变化

测定了烧伤病人及健康成人血和尿中锌、铜、铁、锰、铬的含量。经两两比较，结果表明烧伤病人及其补充微量元素后血锌与铜之间未发生明显变化，Ｐ〉０．０５；而尿锌与铁、锰、铬之间发生变化，Ｐ〈０．０１。     

肺心病与血清锌和铜关系的探讨

对１９５例住院的肺心病患者和９０例健康人分别进行了血清锌、铜的测定，并作了对比分析。结果表明：肺心病患者血清锌较健康人明显下降，血清铜明显升高，且病情愈重，年龄愈大，差异愈大。     

60例非胰岛素依赖型糖尿病人发铬分析

用ＤＣＴ直读光谱仪测定了６０例非胰岛素依赖型糖尿病人发铬微量元素。铬（Ⅲ）含量低于对照组。具有生物活性的铬（Ⅲ）有机化合物－葡萄糖耐受因子（ＧＴＦ）是胰岛素的“协同激素”。铬（Ⅲ）含量降低，葡萄糖耐量受损，可导致胰岛素作用降低，影响糖元的合成与代谢。提示铬的测定对非胰岛素依赖型糖尿病早期诊断及治疗有一定的临床价值。     

High-performance liquid chromatography followed by radioimmunoassay for the determination of a luteinizing hormone-releasing hormone analogue, leuprorelin, and its metabolite

A sensitive method for the determination of leuprorelin (TAP-144), a luteinizing hormone-releasing hormone analogue, and its C-terminal metabolite, M-I, in serum and urine has been developed. Leuprorelin and M-I were extracted from serum or urine samples with Sep-Pak C18 cartridges, and separated completely by high-performance liquid chromatography and determined by radioimmunoassay using [125I]leuprorelin as the labelled antigen. The detection limit of the method was 0.05 ng/ml for leuprorelin and M-I, and the recovery of the compounds added to serum and urine was over 88% with a coefficient of variation (within-assay) of less than 5%. The method was applied to the determination of leuprorelin and M-I-like immunoreactivity in serum or urine after administration of once-a-month injectable microspheres of leuprorelin acetate (TAP-144-SR) to patients with prostate cancer.     

Analytical procedure for the determination of rufloxacin, a new pyridobenzothiazine, in human serum and urine by high-performance liquid chromatography

A high-performance liquid chromatographic method for the quantification of rufloxacin in human serum and urine has been developed and validated. The compounds, rufloxacin and internal standard, are extracted from buffered serum and urine using dichloromethane. They are then separated on an anion-exchange column using 0.05 M phosphate buffer-acetonitrile (80:20, v/v). The eluate is quantified by measuring the ultraviolet absorbance at 296 nm. The lower limit of detection for the analyte is 0.1 microgram/ml in serum and 0.05 micrograms/ml in urine. The method is linear from 0.3 to 10 micrograms/ml for serum and 0.1 to 10 micrograms/ml for urine. The method has been applied in a pharmacokinetic study in volunteers.     

Mix-mode TiO-C18 monolith spin column extraction and GC-MS for the simultaneous assay of organophosphorus compounds and glufosinate, and glyphosate in human serum and urine

A rapid, specific, and sensitive method for the simultaneous quantitation of organophosphates (fenitrothion (MEP), malathion, and phenthoate (PAP)), glufosinate (GLUF), and glyphosate (GLYP) in human serum and urine by gas chromatography-mass spectrometry (GC-MS) has been validated. All of the targeted compounds together with the internal standard were extracted from the serum and urine using a mix-mode TiO-C(18) monolithic spin column. The recovery of organophosphates from serum and urine ranged from 12.7 to 49.5%. The recovery of GLUF and GLYP from serum and urine ranged from 1.9 to 7.9%. The intra- and inter-accuracy and precision (expressed as relative standard deviation, %RSD) were within 96.7-107.7% and 4.0-13.8%, respectively. The detection and quantitation limits for serum and urine were 0.1 and 0.1 μg/ml, respectively, for organophosphates, 0.1 and 0.5 μg/ml, respectively for GLUF and GLYP. The method had linear calibration curves ranging from 0.1 to 25.0 μg/ml for organophosphates and 0.5-100.0 μg/ml for GLUF, and GLYP. The validated method was successfully applied to a clinical GLYP poisoning case.     

Rapid bioanalysis of vancomycin in serum and urine by high-performance liquid chromatography tandem mass spectrometry using on-line sample extraction and parallel analytical columns

A novel high-performance liquid chromatography tandem mass spectrometry (LC/MS/MS) method is described for the determination of vancomycin in serum and urine. After the addition of internal standard (teicoplanin), serum and urine samples were directly injected onto an HPLC system consisting of an extraction column and dual analytical columns. The columns are plumbed through two switching valves. A six-port valve directs extraction column effluent either to waste or to an analytical column. A ten-port valve simultaneously permits equilibration of one analytical column while the other is used for sample analysis. Thus, off-line analytical column equilibration time does not require mass spectrometer time, freeing the detector for increased sample throughput. The on-line sample extraction step takes 15 seconds followed by gradient chromatography taking another 90 seconds. Having minimal sample pretreatment the method is both simple and fast. This system has been used to successfully develop a validated positive-ion electrospray bioanalytical method for the quantitation of vancomycin. Detection of vancomycin was accurate and precise, with a limit of detection of 1 ng/mL in serum and urine. The calibration curves for vancomycin in rat, dog and primate were linear in a concentration range of 0.001-10 microg/mL for serum and urine. This method has been successfully applied to determine the concentration of vancomycin in rat, dog and primate serum and urine samples from pharmacokinetic and urinary excretion studies.     

Determination of cefotaxime and desacetylcefotaxime in plasma and urine by high-performance liquid chromatography

A high-performance liquid chromatographic method is described for the analysis of the anti-bacterial agent cefotaxime and desacetylcefotaxime in physiological fluids. Plasma or serum samples were mixed with chloroform--acetone to remove proteins and most lipid material. The aqueous phase was then freeze-dried, reconstituted in mobile phase and chromatographed on a reversed-phase column using UV detection at 262 nm. Urine was analysed directly after centrifugation to remove particulate matter. The detection limit was 0.5--1.0 micrograms/ml for serum and 5 micrograms/ml for urine. The method has been applied to the analyses of cefotaxime and desacetylcefotaxime in plasma, serum, urine, cerebrospinal fluid, saliva, and pus from infected wound secretions. Two additional metabolites, which are lactones in which the beta-lactam ring has been opened, could be separated by this method.     

Determination of glibenclamide and its two major metabolites in human serum and urine by column liquid chromatography

A simple reversed-phase liquid chromatographic method for the measurement of low concentrations of glibenclamide (glyburide) and its two major metabolites, 4-trans- and 3-cis-hydroxyglibenclamide, in human serum and urine has been developed. The compounds were extracted with n-hexane-dichloromethane (1:1). The UV detection wavelength was 203 nm. The minimum detectable serum level of glibenclamide was 1 ng ml (2 nM), and the relative standard deviation was 8.9% (n = 9). When maximum sensitivity was desired the metabolites were chromatographed separately. Metabolites in urine were measured by the same method after five-fold sample dilution. The utility of the method was tested on a healthy volunteer who ingested 3.5 mg of glibenclamide. The parent drug was present in the serum for at least 18 h, and the metabolites in the urine for at least 24 h.     

Determination of tazobactam and piperacillin in human plasma, serum, bile and urine by gradient elution reversed-phase high-performance liquid chromatography

A gradient elution high-performance liquid chromatographic method is described for the analysis of the beta-lactamase inhibitor tazobactam (YTR-830H) and a semi-synthetic parenteral penicillin, piperacillin, in human plasma, serum, bile and urine. The assay for plasma, serum and bile involves deproteinization with acetonitrile and the removal of lipids with dichloromethane; urine is diluted with buffer. Separation and quantitation are achieved using a mobile phase based on ion-suppression chromatography on a C18 reversed-phase column with ultraviolet detection at 220 nm. The limit of quantitation for both compounds is 1.0 microgram/ml in plasma, serum and bile using a 0.2-ml sample and 50.0 micrograms/ml in urine using a 0.1-ml sample. The method has been validated by preparing and analyzing a series of fortified samples (range 1.0-200 micrograms/ml for each compound in plasma, serum and bile and 50.0-10,000 micrograms/ml for each compound in urine). Excellent linearity, accuracy, precision and recovery were obtained. The method was not interfered with by other endogenous components, nor by other commonly administered antibiotics such as amoxicillin, mezlocillin, cefometazole and cefotaxime. The assay has been successfully applied to the analysis of samples from pharmacokinetic studies in man and animals.     

中毒患者血清和尿液中毒鼠强残留物的GC-MS分析方法

有关资料表明,人和动物口服毒鼠强后,其血液、尿液和各脏器中均有毒鼠强残留物出现,残留时间从药后数小时至几天乃至十几天之内不等。可见血液和尿液作为可印证中毒病人中毒原因的直接样品更值得我们去关注,与呕吐物、可疑食物等检品相比,它具有提取相对简单,干扰成分少,残留时间长以及可反复采集等许多优点。因此,我们结合突发性中毒检验工作的需要,利用超声波液-液萃取技术,研究了中毒患者血清和尿液中毒鼠强残留物的GC-MS-SIM检测方法。在对40多人份血清和尿液添加标准物的反复测定中,回收率血清保持在90.8％～99.5％;RSD为3.82％,尿液保持在91.2％～102.8％,RSD为4.91％,全过程仅需约30min。经过两年来百多份样品检测的验证,该方法不失为日常快速分析中毒患者血清和尿液中毒鼠强残留物的一种有效方法,现介绍如下。     

Simultaneous determination of the sulphonylurea glimepiride and its metabolites in human serum and urine by high-performance liquid chromatography after pre-column derivatization

A sensitive and selective high-performance liquid chromatographic method has been developed for a new sulphonylurea, glimepiride, and its metabolites. The assay involves extraction with diethyl ether, thermolysis of the sulphonylureas at 100 degrees C and trapping of the resulting amines with 2,4-dinitrofluorobenzene. The derivatives were quantitated on a reversed-phase column by absorbance at 350 nm using a step gradient for the three compounds in serum and an isocratic run for the metabolites in urine. Analogous compounds were used as internal standards. The detection limit was 5 ng/ml for glimepiride and metabolite II and 10 ng/ml for metabolite I using 1 ml of serum. The method has been applied to the analysis of serum and urine samples from pharmacokinetic studies in humans.     

A Radioimmunoassay for Serum and Urine Aldosterone by Celite Column Chromatography

Abstract

A relatively simple and rapid radioimmunoassay (RIA) for the measurement of aldosterone in serum and urine has been developed. The method involves extraction of 1 ml of serum or urine (after acid hydrolysis) with dichloromethane, followed by partition chromatography on celite microcolumns prior to RIA. Dextran coated charcoal is used for separation of free from antibody-bound aldosterone. The method is very sensitive, blanks are negligible and recovery is approximately The%. 80 coefficient of variation is 4. 3% (within assay) and 10. 4% (between assay). When known amounts of aldosterone were added to serum and urine pools containing low endogenous levels of this steroid recovery was quantitative. Aldosterone concentrations measured under various physiological conditions were in agreement with published data. Up to 150 samples can be assayed by 1 technician during 5 working days.