手性毛细管色谱法测定人尿中美芬妥英对映体的含量及其在代谢分型中的应用

采用手性毛细管色谱柱和ＦＩＤ检测器建立了人尿中美芬妥英（ＭＰ）对映体的定量分析方法。尿样用二氯乙烷提取，用酸、碱洗涤得以纯化，测得各对映体的最低检测限为６０μｇ／Ｌ。在１１５～６９０μｇ／Ｌ浓度范围内，标准曲线呈良好的线性关系，ｒ＞０．９９，日内、日间精密度ＲＳＤ＜６．５％，Ｓ－ＭＰ的平均回收率为７４．４１％，Ｒ－ＭＰ的平均回收率为７３．７８％。并以ＭＰ为探针药物，对３２名志愿者的尿样进行了ＭＰ氧化代谢分型研究。     

手性毛细管色谱法测定人尿中美芬妥英对映体的含量及其在代谢分型中的应用

 采用手性毛细管色谱柱和ＦＩＤ检测器建立了人尿中美芬妥英（ＭＰ）对映体的定量分析方法。尿样用二氯乙烷提取，用酸、碱洗涤得以纯化，测得各对映体的最低检测限为６０μｇ／Ｌ。在１１５～６９０μｇ／Ｌ浓度范围内，标准曲线呈良好的线性关系，ｒ＞０．９９，日内、日间精密度ＲＳＤ＜６．５％，Ｓ－ＭＰ的平均回收率为７４．４１％，Ｒ－ＭＰ的平均回收率为７３．７８％。并以ＭＰ为探针药物，对３２名志愿者的尿样进行了ＭＰ氧化代谢分型研究。     

高效液相色谱法测定中成药金水清中蜕皮甾酮的研究

本文采用反相色谱液相色谱法（ＲＰ－ＨＰＬＣ）,Ｓｈｉｍ－ｐａｃｋ ＣＬＣ－ＯＤＳ柱,甲醇－水（４０：６０）流动相,在２４８ｎｍ波长处测定中成药金水清中蜕皮甾醇的量。在０．５￣１０００μｇ／ｍＬ范围呈线性关系,相关系数为０．９９９８;方法的检出限为０．１０８ｍｍｏｌ·Ｌ＾－１（Ｓ／Ｎ＝３）,ＲＳＤ为０．６６％（ｎ＝７,Ｃ＝１０．０μｇ／ｍＬ）,采用活性氧化铝柱预分离,以除去主要干扰组分的影响。方法简     

24种安眠镇静药物的气相色谱及气相色谱－质谱系统分析

建立了２４种安眠镇静药物的气相色谱（ＧＣ）及气相色谱－质谱（ＧＣ－ＭＳ）系统分离分析方法。该法在选定的色谱条件下，能将２４种安眠镇静药物很好地分离，互不干扰。采用内标法定量，其线性范围在０～２４μｇ／ｍＬ血，最小检出浓度为０．１～０．４μｇ／ｍＬ血。用所建的ＧＣ方法对１１例中毒病人的生物样品进行分析鉴定，ＧＣ－ＭＳ法验证。从实际中证明所建方法操作简便，准确性和系统性强，灵敏度较高，能快速、准确地为医院的救治提供依据。     

24种安眠镇静药物的气相色谱及气相色谱－质谱系统分析

 建立了２４种安眠镇静药物的气相色谱（ＧＣ）及气相色谱－质谱（ＧＣ－ＭＳ）系统分离分析方法。该法在选定的色谱条件下，能将２４种安眠镇静药物很好地分离，互不干扰。采用内标法定量，其线性范围在０～２４μｇ／ｍＬ血，最小检出浓度为０．１～０．４μｇ／ｍＬ血。用所建的ＧＣ方法对１１例中毒病人的生物样品进行分析鉴定，ＧＣ－ＭＳ法验证。从实际中证明所建方法操作简便，准确性和系统性强，灵敏度较高，能快速、准确地为医院的救治提供依据。     

气相色谱/质谱法测定大鼠脑中5-羟色胺的含量

采用气相色谱／质谱法（ＧＣ／ＭＳ）测定了正常大鼠和服药大鼠脑组织中５－羟色胺（５－ＨＴ）的浓度。大鼠脑组织制成匀浆后,先将５－ＨＴ酰化,酰化物经乙酸乙酯提取后,再经七氟丁酸酐衍生化,用ＧＣ／ＭＳ测定。ＭＳ采用电子捕获负离子化学电离（ＥＣＮＩＣＩ）模式。方法的线性范围为０．５０～５０．０μｇ／Ｌ,回归方程为Ｙ＝０．１３４８Ｘ－０．０７９９５（ｒ＝０．９９９６）;平均回收率为９８．２％±３．８％（ｎ＝１０）;检测限为０．５μｇ／Ｌ;相对标准偏差小于１０％。     

聚乙烯醇对锌镉铅溶出增敏作用及应用

在０．０５ｍｏｌ／Ｌ（ｐＨ６．５）乙二妥－盐酸介质中,聚乙烯醇－１２４ＰＶＡ－１２４）对锌,镉,铅的电位溶出有显著的增敏作用。当富集６０ｓ时,其检出限均达６．０μｇ／Ｌ,线性范围：锌０．６－３５μｇ／Ｌ,镉０．６－４５μｇ／Ｌ,铅０．６－５０μｇ／Ｌ。标准加入回收率为９２．４％－１１０％。ＲＳＤ（ｎ－４）〈７．０％。     

高效液相色谱－荧光检测法测定蒽和荧蒽

采用高效液相色谱－荧光检测法测定多环芳烃化合物蒽和荧蒽。在Ｓｈｉｍ－ｐａｃｋＣＬＣ－ｐｈｅｎｙｌ柱上，以５０％的乙腈水溶液作流动相，１２ｍｉｎ内实现了两组分的同时分离测定。线性范围为０～８０μｇ／ｍＬ，检测限低于５０ｎｇ／ｍＬ，相对标准偏差小于１％。     

高效液相色谱—荧光检测法测定蒽和荧蒽

采用高效液相色谱－荧光检测法测定多环芳烃化合物蒽和荧蒽。在Ｓｈｉｍ－ｐａｃｋ ＣＬＣ－ｐｌｅｎｙｌ柱上，以５０％的乙腈水溶液作流动相，１２ｍｉｎ内实现了两组分的同时分离测定。线性范围为０－８０μｇ／ｍＬ，检测限低于５０ｎｇ／ｍＬ，相对标准偏差小于１％。     

反相高效液相色谱分离—安培法检测酚类化合物

本文报道了ＲＰ－ＨＰＬＣ－安培法检测测定酚类化合物的条件，在Ｓｈｉｍ－ｐａｃｋＣＬＣ－Ｃ８柱上用含０．５ｍｏｌ／Ｌ ＮａＨ２ＰＯ４缓冲溶液的５％甲醇水溶液洗脱分离，于Ｅ＋１．０Ｖ处检测，线性范围在０－７μｇ／ｍｌ，检测限达ｎｇ／ｍｌ。     

Candidate EPA, NIOSH method for determining carbon disulfide in air with capillary gas chromatography by orthogonal design

This paper describes a candidate NIOSH EPA method for the determination of carbon disulfide in the air of workplaces with capillary gas chromatography using an orthogonal design. This method is designed to replace the packed column of the NIOSH method with a capillary column. The first part of this work concerned the setup of the method, particularly the choice of chromatographic parameters and finding their main favorable working ranges. The second part, using the statistical method orthogonal design, focused on optimizing the GC conditions, which were: column temperature, T(c) = 90 degrees C; injector temperature, T(i) = 140 degrees C; U section detector temperature, FPDU = 160 degrees C; L section detector temperature, FPDL = 210 degrees C; flow rate of carrier gas, F(c) = 20 cm/s; split ratio = 1/70; and injection volume = 1 microL. The quality control test showed that the coefficient of intra-day variation (CV) was 2.21%. A good logarithm linear correlation between the standard solutions and their peak areas was obtained. In general, the method reported here seems a valid candidate for a NIOSH EPA method due to its high precision and accuracy.     

Determination and pharmacokinetic study of 1-p-(3.3-dimethyl-1-triazeno) benzoic acid in cancer patients by capillary gas chromatography

A capillary gas chromatographic method was developed for determining 1-p-(3.3-dimethyl-1-triazeno) benzoic acid in the plasma and urine of cancer patients under pharmacokinetic study. The drug was extracted with ethyl acetate and methylated with diazomethane. Octadelane (10 microg/ml) was added as internal standard. The separation was carried out on an OV-1 quartz capillary column, 15 m x 0.32 mm (0.52 microm), with high-purity nitrogen as carrier gas and flame ionization detector (FID) as detector. The column temperature was held at 130 degrees C for 9 min and then programmed to 240 degrees C, at a rate of 35 degrees C/min. The temperature of both injector and detector was 260 degrees C. The standard curve was linear from 0.4 to 40 microg/mL in plasma, and from 0.8 to 20 microg/mL in urine, with correlation coefficients of 0.9979 and 0.9932. The relative standard deviations (RSD) were less than 9.7%. The minimum recovery of this method was 81.8%. This method was applied to the pharmacokinetic studies of 1-p-(3.3-dimethyl-1-triazeno) benzoic acid in cancer patients after a single dose (i.v.) of 160, 420 or 760 mg/m(2) was administered. They all conformed to the two-compartment open model and showed linear pharmacokinetics. The excretion of this drug in the urine was minimal.     

固相萃取-毛细管气相色谱法测定中草药中13种有机氯农药的残留量

建立了中草药中有机氯类农药残留量的固相萃取-毛细管气相色谱(SPE-CGC)分析方法。对丹参、黄芩、射干、白芍、白芷、天南星、牛蒡子、知母、桔梗共9种中草药中六六六的4种异构体、滴滴涕的4种异构体、七氯、艾氏剂、环氧七氯、狄氏剂、异狄氏剂共13种有机氯农药的残留量进行了测定。以丙酮-正己烷混合物作提取剂,采用超声波提取样品,然后用Florisil固相萃取小柱快速净化提取物。采用SPB-5弹性石英毛细管气相色谱柱分离样品,电化学检测器进行检测。13种农药的峰面积与其质量浓度均有良好的线性关系,相关系数均大于0.998。最小检测量为0.064～0.61 μg/L;样品的加标回收率为87.3%～102.3%(相对标准偏差为1.3%～6.8%)。该法简便快速、灵敏准确,具有广泛的应用前景。     

Enantioseparation of ofloxacin in urine by capillary electrokinetic chromatography using charged cyclodextrins as chiral selectors and assessment of enantioconversion

A method was developed for the enantioseparation of ofloxacin, a member of the fluoroquinolones, using an anionic cyclodextrin-derivative with or without combination with a neutral cyclodextrin-derivative, as the chiral selector (s) in an electrokinetic chromatography system. The best results were obtained with 0.35 mM sulfated beta-cyclodextrin dissolved in a 50 mM phosphate buffer, pH 2.5, and at 15 degrees C. Under these conditions, a resolution of 2 was readily achieved. Furthermore, under adequate separation conditions, studies were performed in order to assess possible in vitro and in vivo enantioconversion of levofloxacin. The current method allows detection of 2 microg R-(+)-ofloxacine/mL diluted urine without the necessity of sample cleanup.     

气相色谱法分离和测定3种植物内源激素

 应用大口径毛细管气相色谱法,以正二十二烷为内标物,对植物组织中的吲哚乙酸(IAA)、脱落酸(ABA)和赤霉素(GA)等3种内源激素进行了测定。结果表明:IAA,ABA和GA的最低检测限依次为0.16,0.08和0.48mgL,相对标准偏差均小于3.0%,平均回收率为88.4%～92.2%。方法简便、灵敏、准确、重现性好。     

手性荧光衍生化反相高效液相法分离肾上腺素对映体

 以R (- ) /S (+) 4 (N ,N dimethylaminosulfonyl) 7 (3 iso thiocyanatopyrrolidino) 2 ,1,3 benzoxadiazole(DBD PyNCS)为手性荧光衍生化试剂 ,用反相高效液相法 (RP HPLC)对 DL 肾上腺素对映体进行分离。衍生化反应是在含有 7%吡啶的溶剂中 ,6 5℃温度条件下反应 35min ,生成具有荧光特性的肾上腺素非对映体衍生物(λex=4 6 0nm ,λem=5 5 0nm)。生成的非对映体衍生物在流动相为乙腈 水 (体积比为 2 8∶72 ) ,流速为 1 0mL/min时 ,在DiamonsilTMC18柱 (15 0mm× 4 6mmi d ,5 μm)上分离度可达 2 6。     

Enantioselective determination of the organochlorine pesticide bromocyclen in spiked fish tissue using solid-phase microextraction coupled to gas chromatography with ECD and ICP-MS detection

A method for enantioselective determination of bromocyclen enantiomers in fish tissue has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (CP-Chirasil-Dex CB) and a temperature program from 50 degrees C (held for 1 min), raised to 140 degrees C at 40 degrees C min(-1) and then raised at 0.2 degrees C min(-1) to 155 degrees C. This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on solid-phase microextraction (SPME). Under SPME optimized conditions, precision, linearity range and detection limits of the developed SPME-enantioselective GC procedure were evaluated and compared using two different detection systems: a classical electron-capture detection (ECD) and an element specific detection using inductively coupled plasma mass spectrometry (ICP-MS). The SPME-GC-ECD method exhibited an excellent sensitivity, with detection limits of 0.2 ng L(-1) for each enantiomer of bromocyclen. Although ICP-MS offered poorer detection limits (7 ng L(-1) as Br, equivalent to 36 ng L(-1) of each enantiomer) than conventional ECD detector, it proved to be clearly superior in terms of selectivity. The relative potential and performance of the two compared methods for real-life analysis has been illustrated by the determination of enantiomers of bromocyclen in spiked tissue extracts of trout.     

Solid-phase microextraction in combination with GC-FID for quantification of the volatile free fatty acids in wastewater from constructed wetlands

A headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to flame ionization detector (GC-FID) is developed for the direct determination of volatile fatty acids (VFAs) in wastewater from constructed wetlands. Through the investigation on extraction behavior of different coatings for VFAs and the chromatographic behavior of VFAs in a Stabilwax-DA capillary column (30 mx0.32 mm i.d., 0.25 microm film thickness) using nitrogen as carrier gas, the polyacrylate fiber is selected as the satisfactory coating for VFAs analysis, and optimum chromatographic conditions are obtained. The oven temperature is programmed at 70 degrees C for 2 min, then a 4 degrees C/min rate until 180 degrees C, holding 2 min, and then a 20 degrees C/min rate until 200 degrees C, holding the final temperature for 3 min. The various parameters including extraction time, extraction temperature, pH value, ion strength, sample volume, and desorption conditions are investigated for the optimization of HS-SPME performance for VFAs in the wastewater. The experimental results show that the linear dynamic ranges are 10-45000 microg/L, and over two to four orders of magnitude depending on different acids. The detection limit (3sigma) for VFAs are low to microg/L levels and the relative standard deviations are less than 10%, and the recoveries are between 85% and 117%. By using 2-ethylbutyric acid as internal standard, the proposed method is successfully applied to the determination of VFAs in wastewater from the constructed wetlands.     

气相色谱法直接测定植物生长素

 建立了一种采用 5 3 0 μm大口径毛细管色谱柱、不经衍生化处理而直接测定吲哚乙酸 (IAA)、吲哚丁酸(IBA)和萘乙酸 (NAA)等植物生长素的气相色谱分析方法。以邻苯二甲酸二丁酯为内标物 ,用 FID检测 ,IAA,IBA和 NAA的相对标准偏差分别为 1 .1 4% ,0 .61 %和 0 .78%。方法简便、快速、准确、重现性好 ,可用于生长素类单组分和混合制剂的质量检测。