微量糖缀合物中单糖组成的毛细管气相色谱分离和电子捕获检测

本文介绍了微量糖缀合物中单糖组成的电子捕获毛细管气相色谱分析,讨论了样品组分的分析条件。方法用于测定人脑神经节苷脂、人γ-球蛋白、微生物糖蛋白和植物多糖样品中的糖组分,样品量仅需0.1～5μg。     

气相色谱-电子捕获检测法测定海水中十氯酮残留

通过考察提取溶剂、毛细管柱、净化条件及共溶出干扰物等因素对十氯酮测定的影响,建立了二氯甲烷液-液富集萃取、硫酸净化分离、气相色谱法(GC)-电子捕获检测器(ECD)测定海水介质中有机氯农药类持久性有机污染物十氯酮残留分析方法。1 L海水经50 mL二氯甲烷萃取富集,浓缩后采用硫酸净化,以1%(体积分数)甲醇/正己烷混合溶液转移定容后,采用DB-5非极性毛细管柱进行GC分离,电子捕获检测器可测定其中十氯酮的含量;该方法采用外标法定量,在5～100 μg/L范围内呈线性,线性相关系数为0.9989。低、中、高3个浓度水平的平均加标回收率为81%～108%,相对标准偏差为1.2%～5.1%(n=6)。方法的检出限为0.6 ng/L。结果表明,该方法灵敏度高,线性关系好,可以满足简便、快速、准确测定海水中十氯酮的要求。     

神经节苷脂毛细管电泳的关键分离条件

神经节苷脂毛细管电泳的关键分离条件陈义（中国科学院化学研究所北京１０００８０）关键词毛细管电泳神经节苷脂环糊精神经节苷脂在水溶液中易形成混合胶束［１～３］，通常不被毛细管电泳（ＣＥ）分离。Ｙｏｏ等［４］提出用一级添加剂的方法来促进分离，并发现α－ＣＤ...     

气相色谱／电子捕获检测器法对胶粘剂中卤代烃的测定

胶粘剂样品经乙酸乙酯超声波萃取、过滤后,以三溴甲烷为内标物,采用气相色谱/电子捕获检测器法(GC/ECD)测定其中7种卤代烃的含量.结果表明,该法对卤代烃的定量下限为0.005～2 mg/L,样品加标回收率为95%～102%.4个实验室对氯丁胶中卤代烃测定的相对标准偏差为2.5%～4.2%.     

气相色谱-电子捕获检测法和气相色谱-质谱法同时测定鱼体内19种有机氯农药

建立了气相色谱-电子捕获检测(GC-ECD)法同时测定,及气相色谱-离子阱-多级质谱(GC-IT-MS/MS)法定量确证鱼体中19种有机氯农药(OCPs)残留的检测方法。目标物采用浸渍-振荡法提取,固相萃取(SPE)(脂肪含量≤1.0%)和凝胶色谱(GPC)净化,浓缩,定容后上机测定。草鱼肌肉空白组织中目标化合物的添加浓度为2.0、5.0μg/kg时,GC-ECD法与GC-IT-MS/MS法的回收率分别为72.8%～96%和78.8%～106%,相对标准偏差分别为2.1%～14.9%和4.8%～11%。定量限(S/N=10)分别为0.07～1.44μg/kg和0.10～4.27μg/kg。本方法已成功应用于长江圆口铜鱼体中多种OCPs残留的同时测定。     

气相色谱-电子捕获检测器同时测定硝基咪唑类药物

建立了气相色谱-电子捕获检测器同时测定硝基咪唑类药物含量的方法.样品用磷酸盐调节pH约为8.8,乙酸乙酯提取,无水硫酸钠脱水.采用CBP-1毛细管柱分离,电子捕获检测器检测.甲硝唑、替硝唑、奥硝唑分别在0.2～15 μg/mL、5.3～53μg/mL、4.0～40μg/mL范围内与峰面积呈良好线性关系,相关系数r分别为0.9993、0.9996、0.9995.样品加标回收率在95.8%～101%之间,相对标准偏差在1.8%～3.4%之间.本法简便、快速,可用于片剂和注射液中硝基咪唑类药物含量的测定.     

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...     

气相色谱/电子捕获检测法测定键合态糖苷的研究

该文建立了GC/ECD法测定键合态糖苷的分析方法,采用N-甲基-双(三氟乙酰胺)(MBTFA)对目标物进行衍生,并优化了反应温度和时间.结果表明在60℃下反应50 min时,衍生效果最好.该衍生反应在产物中引入氟元素,可用GC/JECD法进行测定.以苯氧基葡萄糖苷为典型目标物进行线性研究,方法在0.05～200 mg/...     

牛颌下腺粘蛋白中糖组成的毛细管气相色谱分析

根据各种糖革键稳定性的差异，采用没的酸解方法，使各种单糖从牛颌下腺粘蛋白上游离下来。纯化后衍生成三甲基硅醚或糖醇乙酸酯，应用毛细管气相色谱技术分析。结果表明，牛颌下腺粘蛋白中含三类糖，即唾液酸、中性糖和氨基糖。每咱单糖的含量分别为５－Ｎ－乙酰神经氨酸４．３％；５－Ｎ＝乙醇酰神经氨酸１９．０％；岩藻糖３．２％；半乳糖５．１％；Ｎ－乙酰氨基半乳糖１８．４％；Ｎ－乙酰氨基葡萄糖８．７％。     

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.     

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。     

A Study on Effective Derivatization for Ultra-Micro Detection of Dopamine by Gas Chromatography / Electron Capture Negative Ion Chemical Ionization Mass Spectrometry

Abstract

N-Pentafluorobenzenesulfonyl-O-bis (trimethylsilyl) dopamine was prepared and its properties were discussed for ultra-micro detection of dopamine by gas chromatography / electron capture negative ion chemical ionization mass spectrometry (GC/ECNICIMS). Detection of this derivative was at least 100 times as sensitive by GC/ECNICIMS as by gas chromatography / positive ion chemical ionization mass spectrometry. Deuterium labelled dopamine, dopamine analog phenethylamine and deuterium labelled phenethylamine were also derivatized, respectively, to reveal the fragmentation mechanism of the dopamine derivative. the high sensitivity and speculated fragment ion composition of the derivative by GC/ECNICIMS showed a possibility for highly sensitive detect ion of dopamine.     

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.     

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。     

Determination of Pesticides in the Rhizome of Traditional Chinese Medicines by Gas Chromatography with Electron Capture Detection

A simple and efficient gas chromatography method for the determination of 27 organochlorine and pyrethroid pesticides in traditional Chinese medicine was developed. Pesticide residues were extracted from the samples by oscillation and ultrasound, and purified by gel permeation chromatography and florisil solid phase extraction. The analysis was performed by gas chromatography with micro-electron capture detection. The purification conditions, such as the extraction and elution solvents, extraction methodology, and gel permeation chromatography conditions, were optimized. Traditional Chinese medicines were purified by different methods based on their composition. Under optimized conditions, the calibration graph was linear from 10 to 500 µg/L and the correlation coefficients varied from 0.9958 to 0.9997. The detection limits of these pesticides were between 0.09 and 1.82 µg/kg. The recovery of the pesticides spiked in various samples at four concentrations ranged from 73.2% to 106.4%, with relative standard deviations between 1.0% and 14.0%. This study indicates that the method is useful for determining pesticides in rhizome traditional Chinese medicines.