有机溶剂对某些有机磷农药的NECC洗提影响的研究

以有机磷农药甲基对硫磷、对硫磷等为被试验物质，探讨了在十二烷基硫酸钠、硼砂电解液中加入甲醇、乙醇、异丙醇、乙腈等有机溶剂对某些有机磷农药的毛细管胶束电动色谱分离的影响，并从电解液的物理化学性质和毛细管色谱动力学两方面阐明了其影响机理。     

毛细管电泳和火焰光度检测器的联用研究

研究了毛细管电泳与火焰光度检测器的联用技术及其应用。有机磷农药经毛细管电泳分离后，流出液被引入气相色谱的火娄光度检测器进行特效检测，毛细管电泳的接地电极接口采用毛细管裂缝处裹醋酸纤维膜的方法，而毛细管电泳和火焰光度检测器的接口则借用了气相色谱的进样口。     

气相色谱-串联质谱法同时测定白芍中10种有机磷农药残留

建立了同时测定中药白芍中10种有机磷农药残留含量的气相色谱–串联质谱方法。样品用乙腈超声提取,提取液经凝胶渗透色谱净化后,以VF–5毛细管色谱柱(30 mm×0.25 mm,0.25μm)分离,串联四极杆质谱仪为检测器进行定性、定量分析。10种有机磷农药残留的检出限为0.02～4.0 mg/kg,实际样品的加标回收率为75%～105%,相对标准偏差为4%～10%。该方法能够满足白芍中有机磷农药残留的定性、定量检测要求。     

毛细管气相色谱法测定韭菜中13种有机磷农药残留的研究

建立了毛细管气相色谱法测定韭菜中敌敌畏、甲胺磷、乙酰甲胺磷、甲拌磷、氧化乐果、久效磷、乐果、毒死蜱、甲基对硫磷、马拉硫磷、杀螟硫磷、对硫磷和喹硫磷等13种有机磷农药残留的新方法.考察了进样口压力和程序升温速率对色谱分离的影响.试样用乙腈提取,经毛细管气相色谱柱DB-1701(30 m×0.32 mm×0.25 μm)分离,FPD检测器测定.当进样口压力为68.9 kPa,程序升温速率为5 ℃/min时,13种有机磷农药与韭菜基质在30 min内获得有效分离.添标水平为0.05、0.2 mg/kg时的平均回收率为78% ～115%,相对标准偏差为2.6% ～10.7%,方法检出限(S/N=3)为0.01 ～0.03 mg/kg,符合农药多残留定性、定量分析技术的要求.     

多种有机磷农药残留量的毛细管气相色谱分析

从目前的发展看,毛细管气相色谱是唯一能满足多种农药残留量对灵敏度和分离能力要求的分析手段。国外已有一些这方面的研究报告,但国内尚未见有关的报道。我们在这方面进行了研究,采用岛津GC-9A气相色谱仪及其毛细管柱附件,对其载气控制及进样部分进行了改造,建立了一套实用的多种有机磷毛细管气相色谱分析方法,可同时检测水果、蔬菜等低脂肪含量样品中20种以上的有机磷农药残留量,最低N_2检出量为2～20ppb。     

果实类中药材中20种有机磷农药残留量的同时测定

建立了果实类中药材中多种有机磷农药残留同时测定的方法,并对影响提取、净化、检测效率的因素进行优化。样品用乙酸乙酯提取,凝胶渗透色谱收集9~15 min流分,ENVI-Carb固相萃取柱净化,DB-1701毛细管色谱柱分离,火焰光度检测器检测,外标法定量。在优化条件下,20种有机磷农药在0.01~2.0mg/L范围内具有良好的线性关系,相关系数为0.996 6~0.999 5,检出限(S/N=3)为0.66~5.78μg/kg。3个加标水平下的平均回收率为80.2%~109.9%,相对标准偏差为2.3%~13%。该方法操作简便、准确、净化效果好,可满足果实类中药材中多种有机磷农药残留的同时测定要求。     

超性能石英毛细管色谱柱的研制及有机磷农药残留量的分析

采用三种端痉基聚硅氧烷试剂对石英毛细管进行钝化处理，考察了钝化处理的石英毛细管与不同极性固定相的润湿性。在脱活试剂中加入二丁基二月桂酸锡催化剂，降低了钝化反应温度，从而制备出了超性能的石英毛细管色谱柱，在有机磷农药残留量的分析中取得了满意结果。     

8种农药的大口径毛细管气相色谱分析

1　引　　言2 0世纪 80年代 ,毛细管气相色谱 (CGC)技术就广泛用于农药残留分析。现在毛细管气相色谱与固相萃取、固相微萃取、质谱等技术一起 ,被广泛地应用于农药的多残留分析。但作为农药原药和制剂的有效成分的常规分析 ,直至进入2 0世纪 90年代后才在农药国际标准分析方法 (CIPAC)手册中相继出现。近年来 ,随着大口径毛细管推广应用和一些重大技术的改进 ,毛细管气相色谱作为农药的常规分析方法 ,发展比较快。到目前为止 ,CIPAC已经建立了近 2 0个农药原药及其制剂的毛细管气相色谱标准分析方法。大口径毛细管气相色谱法具有分析…     

果蔬中107种残留农药的气相色谱-质谱检测方法

采用毛细管气相色谱-质谱法对果蔬中107种残留农药检测进行了系统研究,考察了被测组分在不同极性毛细管色谱柱上的保留时间值,对比了不同前处理技术对检测结果的影响,确定了气相色谱-质谱检测农残初筛离子选择原则,规定了气相色谱-质谱确证被捡出农药应符合的条件。     

水中重点有机磷农药的毛细管气相色谱法测定

研究建立了气相色谱－火焰光度检测器（GC－FPD）法测定水中14种有机磷农药的分析方法,在选定的色谱条件下,14种有机磷农药在18min内得以很好的分离。在该方法下,14种有机磷农药的精密度良好,其中12种有机磷农药的加标回收率为92％－114.6％。     

DB-1701柱分离测定水中六种有机磷农药

采用低毒性的正己烷简便萃取水中敌敌畏、敌百虫、乐果、甲基对硫磷、马拉硫磷及对硫磷,使用DB-1701石英毛细柱,用程序升温气相色谱法测定。能实现6种农药较好分离,实验结果能满足气相色谱分析要求,且相关参数比标准和有关资料的数据有所提高,增加了检测的准确性和灵敏度。     

固相萃取–气相色谱法测定饮用水中5种有机磷农药

建立了固相萃取–气相色谱法测定饮用水中敌敌畏、乐果、甲基对硫磷、马拉硫磷及对硫磷的方法。采用Cleanert PEP–SPE固相萃取柱,以二氯甲烷、乙酸乙酯、甲醇及纯水活化固相萃取柱,以5 m L/min流量富集水样,然后用二氯甲烷及乙酸乙酯洗脱浓缩后进行气相色谱分析。5种有机磷农药线性相关系数均大于0.995,方法测定下限为0.16~0.80μg/L,加标回收率为59.8%~109.0%,测定结果的相对标准偏差小于16%(n=6)。该方法灵敏度高,准确度好,适用于饮用水中5种有机磷农药的检测。     

Fluorescence observation supporting capillary chromatography based on tube radial distribution of carrier solvents under laminar flow conditions

We developed a capillary chromatography system by using an open capillary tube made of fused-silica, polyethylene, or polytetrafluoroethylene, and a water-hydrophilic/hydrophobic organic mixture carrier solution, called tube radial distribution chromatography (TRDC) system. By comparing with chromatograms obtained via the TRDC system, fluorescence photographs and profiles of the fluorescent dyes dissolved in the carrier solvents in capillary tubes were observed under laminar flow conditions. The chromatograms were obtained for a model mixture analyte consisting of 1-naphthol and 2,6-naphthalenedisulfonic acid with the TRDC system, by using a fused-silica capillary tube and a water-acetonitrile-ethyl acetate carrier solution. By altering the carrier flow rates, we examined the fluorescence photographs and profiles of the dyes, perylene and Eosin Y, dissolved in the carrier solvents in the capillary tube by using a fluorescence microscope equipped with a CCD camera. As confirmed by fluorescence observations, the major inner and minor outer phases generated in the capillary tube were based on the tube's radial distribution of the carrier solvents. We designed and manufactured a microreactor incorporating microchannels in which three narrow channels combined to form one wide channel. When the carrier solvents containing the dyes were fed into the channels, the inner and outer phase generations were also observed in the narrow and wide channels, strongly supporting the conclusions concerning the tube radial distribution phenomenon of the solvents.     

Tentative Comparison of Tube Radial Distribution Chromatography and CZE

Tube radical distribution chromatography (TRDC) uses an untreated open tubular capillary tube and a ternary mixture of solvents (water and hydrophilic/hydrophobic organic solvents) as a carrier solution. A model analyte mixture comprising 1-naphthol, 1-naphthoic acid, 1-naphthalenesulfonic acid, 2,6-naphthalenedisulfonic acid, and 1,3,6-naphthalenetrisulfonic acid was examined by the TRDC and capillary zone electrophoresis (CZE) systems that comprised mainly a capillary tube and a detector. In the TRDC system the elution order of analytes could be changed by altering the component ratios of the solvents, whereas in the CZE system the elution order was changed by altering the electroosmotic flow direction. The experimental data obtained provide clues about the features and utility of TRDC as a new separation method.     

Extraction of pesticides from aqueous samples: A comparative study

Three different extraction procedures for eight pesticides (chlorfenvinphos, diazinon, ethyl parathion, ethiofencarb, fenitrothion, malathion, metalaxyl, pirimicarb) in water samples are compared. The extraction procedures are: liquid-liquid extraction (LLE), solid-phase extraction (SPE) and microextraction (ME). For each procedure the most suitable conditions were obtained experimentally, with special remarks on ME, in which the effects of different mixtures of Kaltron with other solvents were tested. A preconcentration factor (PF) was used to rank the methods; the best results were observed for ME, (PF 15–45, whereas PF < 10 for SPE, and PF 13 for LLE). In all cases, the determination was performed by gas chromatography, using a nitrogen phosphorus detector and the internal standard method (methyl parathion) as the quantification procedure.     

微波辅助萃取/气相色谱-质谱联用分析蔬菜中的有机磷农药

建立了微波辅助萃取（MAE）/气相色谱-质谱联用法（GC-MS）测定蔬菜样品中二嗪磷、水胺硫磷的分析方法，研究了不同溶剂的萃取效率。选择二氯甲烷为萃取溶剂，采用二因素三水平的正交设计实验优化了萃取溶剂体积和萃取时间。方法的线性范围分别为二嗪磷和对硫磷4ng/g-400ng/g，水胺硫磷20ng/g-400ng/g，检出限分别为二嗪磷和对硫磷4ng/g-400ng/g、水胺硫磷20ng/g-400ng/g，检出限分别为二嗪磷0.29ng/g、对硫磷1.70ng/g、水胺硫磷2.30ng/g。测定200.0ng/g和50.0ng/g加标蔬菜样品，回收率为72.2%-102.0%,RSD为1.5%-11.0%。与传统的机械振荡萃取法相比，不仅萃取效率相当，而且还具有省时省溶剂的优点。     

Separation of chlorins and carotenoids in capillary electrophoresis

The present study reports the investigation of capillary electrophoresis (CE) for the separation of the photosynthetic pigments (chlorophyll derivatives as well as carotenoids) together. Various CE methods, such as micellar electrokinetic chromatography, capillary electrokinetic chromatography, and nonaqueous capillary electrophoresis (NACE) are tested, with coated and uncoated capillary columns to evaluate optimal separation conditions using diode array detection. The effect of different type and composition of organic solvents and surfactants on the separation is discussed. Detection limits are found in the range of 1.14-2.45 ppm. According to the system suitability results, the most effective separation is observed using NACE with Aliquat 336 as cationic surfactant in coated capillary and mixture of MeOH-ACN-THF (5:4:1, v/v/v) as solvent. Quantitative evolution is investigated, and recovery percentage values are found to be 96.7-102%.     

Combination of hollow‐fiber‐supported liquid membrane and dispersive liquid–liquid microextraction as a fast and sensitive technique for the extraction of pesticides from grape juice followed by high‐performance liquid chromatography

The simultaneous use of a hollow‐fiber‐supported liquid membrane and dispersive liquid–liquid microextraction for the determination of pesticides directly in grape juice was investigated. The detection and quantification were performed by liquid chromatography with diode array detection. The optimum extraction condition was reached by filling the pores of the membrane wall with dodecanol and using hexane/acetone as extraction/dispersion solvents. Salt addition had a highly negative effect on the extraction efficiency and the optimum extraction time was 60 min. The volume of hexane/acetone mixture and the sample pH did not affect the signal at the levels studied. Therefore, an intermediate amount of these solvents (250 μL; 1:7.5 v/v) and pH 6 were selected. The optimum desorption condition was obtained with acetonitrile and 10 min of desorption time. The linear working range varied from 58 to 500 μg/L (parathion‐methyl), 62–500 μg/L (difenoconazole) and 107–500 μg/L (chlorpyrifos), with correlation coefficients ranging from 0.9980–0.9942. The limits of detection and quantification found were, respectively, 17 and 58 μg/L for parathion‐methyl, 19 and 62 μg/L for difenoconazole and 32 and 107 μg/L for chlorpyrifos. The relative standard deviation ranged between 3.5 and 11.2%.     

固相萃取–毛细管气相色谱法同时测定水体中8种有机磷类农药残留

建立固相萃取–毛细管气相色谱法同时测定水体中敌敌畏、乙酰甲胺磷、治螟磷、乐果、甲基对硫磷、马拉硫磷、杀螟硫磷和水胺硫磷8种有机磷类农药残留。样品经OASIS HLB固相萃取柱富集,丙酮洗脱,用毛细管气相色谱(FPD)法进行定量分析。8种有机磷类农残留的质量浓度在0.05~4.0μg/m L范围内与色谱峰面积线性关系良好,相关系数均大于0.998,方法检出限为0.004~0.01μg/m L。测定结果的相对偏差为2.6%~4.5%(n=6),加标回收率为81.6%~106.2%。该方法操作简单、灵敏度高,可用于检测水体中的8种有机磷类农药残留。     

室温离子液体在色谱分离中的应用进展

室温离子液体作为21世纪的新型溶剂,近几年在分析领域应用广泛.本文重点综述了离子液体在气相色谱、液相色谱、毛细管电泳及薄层色谱等方面的应用进展,并对其在色谱分离中的研究进行了展望.