Determination of Aromatic Amines in Textile After Bromination, by Gas Chromatography Coupled with Electron Capture Detection

A new analytical method is developed for the improved determination of banned aromatic amines in textiles based on the bromination of the aromatic ring system to yield the corresponding bromo derivatives. The derivatization method is very easy to perform and the derivatives can easily extract and separate with gas chromatography. Due to the introduction of the electron withdrawing bromo substituents sensitive detection with very low limits of detection using an electron capture detector is possible. The method was optimized and used for the analysis of textile with quantitative recoveries from spiked samples.     

A Comparison of Some Derivatives of Primary Amines for Gas Chromatography Using Electron Capture Detection

Abstract

Thirteen derivatives of phenethylamine were prepared. The sensitivities of flame ionization and electron capture detectors to these compounds and the original amine were determined. All compounds showed approximately the same sensitivity of detection with a flame ionization detector, but with an electron capture detector there was a 2 × 10⁵ difference in sensitivity of detection between the derivatives showing the greatest and the least sensitivity. The derivative with the greatest sensitivity of detection was the pentafluorobenzaldehyde-amine condensation product and amounts of the amine down to 10 picograms could easily be quantified.     

Electron Capture Gas Chromatography of Nitrazepam in Human Plasma as Methyl Derivative

Abstract

A method for quantitative determination of nitrazepam in human plasma in the range 5 - 100 ng/ml is presented.

Nitrazepam is extracted with benzene from plasma samples of 0.5 ml, methylated with methyl iodide and determined gas chromatographically with an electron capture detector of ⁶³Ni-type.

Acid dissociation constants of nitrazepam are determined and the partition properties studied with benzene, methylene chloride and diethyl ether as organic phases.

The selectivity of the method with respect to the metabolites has been thoroughly studied.     

气相色谱电子捕获检测器检测蟑螂头部痕量章鱼胺的衍生物

章鱼胺(OA)是昆虫体内的痕量神经活性物质。本实验研究了蟑螂头部基质中OA的提取、章鱼胺与五氟丙酸酐的衍生化反应,优化了最佳衍生反应条件。建立了适合于昆虫样本中OA痕量测定的衍生化气相色谱-电子捕获检测方法。昆虫头部匀浆样本在10 ng/g OA添加浓度时回收率在89%~118%;该方法的最低检出浓度为1.7ng/g。采用GC-MS对衍生化产物进行了定性确证分析。     

气相色谱法测定溴己新血药浓度及药代动力学研究

建立了人血浆中溴己新的气相色谱 电子捕获测定法 ,对溴己新胶囊在健康人体内的药代动力学进行了研究。色谱柱为 5 %SE 30 (2m× 3mmi.d .)硅烷化玻璃柱。 5 氯 2 氨基二苯甲酮为内标 ,血浆样品加入磷酸盐缓冲液 (pH 6 0 )后用正己烷 二氯甲烷 (体积比为 9∶1)提取。线性范围为 1 0 μg/L～ 5 0 0 μg/L ,r =0 9994。人血浆中最小检测质量浓度为 0 5 μg/L。方法重现性好 ,日内、日间RSD分别小于 4 5 6 %和 7 11% ,平均回收率 97 5 %。 8名健康志愿者口服 8mg溴己新胶囊后 ,其体内代谢过程符合一房室模型。方法可用于体内血药浓度测定 ,简单、快速 ,灵敏度高 ,数据准确可靠     

气相色谱法测定禽蛋中微量有机氯农药及多氯联苯的残留

建立了以正己烷振荡提取，以及PCB2和PCB209为内标的快速检测禽蛋中微量有机氯污染物的气相色谱法。与传统的索氏提取法相比，在保证足够的准确度，精确度和灵敏度的前提下，具有前处理简单，测试成本低，标本用量少的特点。而且可同时测定有机氯农药和典型的多氯联苯类化合物的残留，特别适于检测食品中的微量有机污染物。用该方法测试的结果表明，标准全蛋粉添加ng/g级待测物时，各种待测物的回收率为84．31％－116．77％（3次测定平均值）；相对标准偏差为6％－18％（7次测定平均值）；最低检出量为0.07ng/g-0.35ng/g。中国部分城市市售鸡蛋中的有机氯农药以p,p'-DDE的检出量最高，p,p'-DDT次之；多氯联苯的检出量很低，大多数样品中多氯联苯的总检出量低于10ng/g。在所检出的多氯联苯中，绝大部分为含氯低的（氯原子数为3－5）的氯化物。     

气相色谱-电子捕获法测定血浆中的雷公藤甲素

 血浆样品经碱化后用乙醚 氯仿 (体积比为 3∶1)混合液提取 ,浓缩的提取物与三氟醋酐进行衍生化反应 ,用气相色谱法分离、63Ni电子捕获检测器测定雷公藤甲素的含量。色谱柱为SE 5 430m× 0 2 5mmi d 交联石英毛细管柱。雷公藤甲素的质量浓度在 1 0 μg/L～ 5 0 0 μg/L范围内与峰面积线性关系良好 (r =0 9990 ) ,在血浆中的平均回收率为 96 3% ,最小检测限为 0 5 μg/L。方法重现性好 ,准确、灵敏 ,无杂质干扰 ,数据准确可靠 ,可用于临床生物样品中雷公藤甲素含量的测定。     

Precolumn,Capillary Column,Electron Capture G-AS Chromatography For High Efficiency Trace Determination

Abstract

A method for gas chromatographic trace determination is described in which the sample solution is injected into a packed precolumn which is connected to an EC-detector. When solvent and low boiling compounds have been eluted, the precolumn is connected to the cold entry of a capillary column with another EC-detector and the trace compound is collected as a narrow band at the entry of this column. The precolumn is then reconnected to its own detector, the capillary column is heated and the trace compound is eluted and measured. Meanwhile high boiling compounds are swept out of the precolumn. When the base line of the precolumn is stable the next sample is injected and the capillary column is cooled again, and so on. In order to avoid background plateaus and ghost peaks the carrier gas must be purified, which is easily achieved with cooling traps with dry-ice and acetone.     

Correlation between Electron Capture Response and Chemical Structure for Sulfur Compounds

Abstract

The temperature dependence of the electron capture process was investigated for a series of divalent sulfur compounds. The electron affinity and/or the activation energy for the electron capture reaction were calculated for individual compounds by plotting In KT^3/2 vs. 1/T, where K is the electron capture coefficient and T is the absolute temperature in the detector. The correlation between these values and chemical structure was discussed by means of 3d orbital resonance of the sulfur atom.     

Electron Capture Determination of Propoxyphene from Human Plasma

Abstract

A procedure for the determination of propoxyphene (α-d-dimethylamino-1, 2 -diphenyl-3 -methyl-2 -propionoxybutane) in plasma is reported. The method is based on the electron capture characteristics of propoxyphene. The plasma is rendered basic to generate the free amine and extracted with ether. The extract is analyzed by gas chromatography using a 4 foot OV-225 column. An internal standard of imipramine hydrochloride is used to quantitate the propoxyphene. This internal standard is carried through the entire procedure. The ratio of the peak heights of propoxyphene to imipramine is compared to ratios obtained from standards placed in plasma and treated in the same manner as the samples. Six subjects were given propoxyphene at different time intervals, and the data are presented concerning these subjects.     

植物源食品中6种三唑类杀菌剂残留量的气相色谱法测定

建立了同时测定6种三唑类杀菌剂(四氟醚唑、戊菌唑、氟菌唑、己唑醇、丙环唑、氟环唑)残留量的气相色谱方法.植物源食品采用乙腈溶剂提取,无水硫酸镁、氯化钠盐析,经弗罗里硅土固相萃取柱净化后,用气相色谱/电子捕获检测器(GC/ECD)测定.结果表明:6种三唑类杀菌剂在0.01 ～0.5 mg/L范围内线性关系良好,相关系数均大于0.996,样品添加水平为0.05 ～0.20 mg/kg时的平均加标回收率为87% ～110%,相对标准偏差为3.0% ～5.6%,方法的检出限为0.002 ～0.007 mg/kg.该方法可同时满足植物源食品中多种三唑类杀菌剂残留量的检测需要.     

气相色谱-电子捕获检测法直接测定水产动物组织中五氯苯酚及其钠盐

建立了不经衍生直接测定水产动物组织中五氯苯酚及其钠盐残留量的气相色谱-电子捕获检测(GC-ECD)方法.目标化合物在酸性条件下转化成五氯苯酚后用正己烷提取,硫酸磺化法净化,浓缩和定容后测定.方法的线性范围为0.5～400 μg/L,相关系数为0.9978;草鱼和虾空白肌肉组织中添加五氯苯酚的质量浓度分别为0.4、2.0...     

Electron Capture Gas Chromatographic Assay for Miconazole and Clotrimazole In Skin Samples

Abstract

Electron capture gas chromatographic assay procedures were developed for quantitating the antifungal agents clotrimazole and miconazole. The procedures were specifically developed for analysis of the drugs in superficial samples of human skin. The analytical methods were sensitive to 5 ng of miconazole and 10 ng clotrimazole per tissue sample.     

气相色谱-质谱法同时测定番茄制品中拟除虫菊酯类农药残留

番茄制品经乙腈提取,盐析,氟罗里硅土固相萃取小柱净化,微池电子捕获检测器(μECD)负化学源质谱(NCI—MS)并联对净化液进行检测,一次进样可对番茄制品中的9种拟除虫菊酯类农药残留准确定量和确证。μECD回收率为87．6％～107．0％;相对标准偏差为5．5％～11．3％;检出限为0．0005～0．005mg／kg;负化学源选择离子(NCI-SIM)模式回收率为91．9％～109．7％;相对标准偏差为5．2％～12．7％;检出限为0．0005～0．005mg／kg(氯菊酯除外),两者之问没有显著的差别。该法快速、灵敏、准确,各项技术指标均满足农药残留检测的要求。     

Testosterone Heptafluorobutyrates: Derivatives for Gas Chromatography

Abstract

The reaction of testosterone with heptafluorobutyric anhydride, in the presence of pyridine or collidine, leads to two diheptafluorobutyrate (HFB) derivatives. These compounds are believed to be the di-HFB esters of 2,4-androstadien-3, 17β-diol (A) and 3, 5-androstadien-3, 17β-diol (B), with A as the major product. This is similar to the reaction with silylating reagents which leads to two isomeric enol ethers. In benzene or acetone solution, and in the absence of an organic base, the same two isomers are formed, but with B as the major product. Although the latter reaction has been recommended for quantitative work, the formation of isomeric enol esters has not been noted. Since the products are not stable in the reaction medium, the method is not entirely satisfactory. The reaction in pyridine solution should be suitable for quantitative work; the products are stable in solution and can be detected in subnanogram amounts.     

丹酰氯柱前衍生仲胺的高效液相色谱-电化学检测方法的研究

立了一种灵敏检测仲胺的新方法。首次以丹酰氯作为仲胺的电化学检测衍生试剂,对分离检测条件、仲胺的衍生条件及电化学定量检测条件作了详细的研究。以甲醇－２０ｍｍｏｌ／Ｌ的邻苯二甲酸氢钾缓冲液（７０∶３０,ｐＨ３．３）为淋洗液,采用安培检测器在Ｅ＝＋１．１Ｖ电压条件下,在ＰＥＲＫＩＮ－ＥＬＭＥＲ／ＨＳ－３Ｃ１８（８３ｍｍ×４．６ｍｍｉ．ｄ．,３μｍ）柱上实现了二甲胺、二乙胺和哌啶的良好反相分离和灵敏检测,线性范围超过两个数量级。二甲胺、二乙胺和哌啶的检出限分别为０．０２４,０．６０,０．０９０ｐｇ。     

不同氯代毒杀芬的全二维气相色谱分离分析方法研究

建立了全二维气相色谱-电子捕获检测器法(GC×GC-μECD)分离分析不同氯代毒杀芬的新方法。通过实验优化,以非极性的DB-1MS为第1根色谱柱,以中等极性的BPX-50为第2根色谱柱对工业毒杀芬不同氯代化合物进行分离分析,获得良好的分离效果。采用基质曲线外标法进行定量分析,线性系数(r2)均大于0.99,不同氯代毒杀芬的检出限(S/N=3)为0.2~0.6μg/L,相对标准偏差(RSD,n=7)为9%~20%,利用土壤为基质进行加标实验,不同氯代毒杀芬同类物的回收率为65%~105%。     

全二维气相色谱-电子捕获检测器法分析土壤中毒杀芬同类物的残留

建立了全二维气相色谱-电子捕获检测器(GC× GC-μECD)检测土壤中毒杀芬同类物的分析方法.以非极性的DB- XLB(20 m×0.25 mm×0.25 μm)为第一色谱柱,中等极性的BPX-50(2 m×0.1 mm×0.1 μm)为第二色谱柱,对土壤中23种高关注毒杀芬同类物进行了分离鉴定,并采用基质曲线外标法进行定量分析.本方法在1～200,μg/L浓度范围内,毒杀芬同类物的线性相关系数(r2)均大于0.99,方法检出限(S/N=3)为0.039～0.482 μg/L,基质加标毒杀芬同类物的回收率为55％～115％,相对标准偏差(RSD)均小于30％(n=5).利用本方法对毒杀芬污染的土壤样品进行了测定,获得了较好的分离效果.