毛细管内固相微萃取技术的研究进展

毛细管固相微萃取技术作为一种新型微萃取技术,与其他固相微萃取技术比较具有萃取效率高、固定相种类丰富、易于与其他分析技术联用等优点。本文主要综述了毛细管内固相微萃取技术的萃取模式、固定相制备、萃取参数优化及与色谱在线联用情况。     

分子印迹整体材料在固相萃取中的应用及展望

分子印迹整体柱结合了分子印迹技术高的分子识别选择性能和整体柱制备过程简单、易于修饰改性、重复性好以及传质速度快等优点,是固相萃取和固相微萃取技术的发展趋势和前沿课题之一.主要介绍了分子印迹聚合物整体材料在与高效液相色谱和毛细管液相色谱法联用技术方面的应用,以及在固相微萃取中的应用,展望了分子印迹整体材料在固相萃取方面的发展趋势.     

固相微萃取——气相色谱法测定污水中的苯系物

采用固相微萃取(SPME)和气相色谱(GC)技术对污水中苯系物进行了分析测定.针对要检测的几种苯系物,采用100μm聚二甲基硅氧烷(PDMS)作为固相微萃取(SPME)装置的固相涂层,并对SPME的参数进行了优化.本方法的重复性好,相对偏差＜5%;线性范围较宽,在0.10～10.0μg/L浓度范围;色谱峰面积与溶液浓度具有良好的线性关系,相关系数＞0.997;检测限均低于0.07μg/L;回收率为88.3%～114.0%.     

地表水中有机磷农残测定的前处理方法比较

分别采用液液萃取法和固相萃取法提取地表水样品中的有机磷农药残留。液液萃取法的方法检出限为0.05~0.2 ng/mL,加标回收率为86%~103%,相对标准偏差为2%~7%;固相萃取法的方法检出限为0.03~0.05 ng/mL,加标回收率为49%~118%,相对标准偏差为5%~18%。液液萃取法处理不同类型基体水样的测试稳定性较好,固相萃取法则对于洁净环境水体中痕量有机磷农药残留的富集更为适用。     

乙酰甲胺磷分子印记聚合物制备及其在农残检测分散固相萃取中的应用

随着人们对食品安全的不断关注,食品中的农药残留检测越来越受到重视,本文以乙酰甲胺磷为模板分子,通过悬浮聚合法制备出分子印迹聚合物(MIP),采用固相微萃取前处理技术[1],结合气相色谱,建立了对茶叶中乙酰甲胺磷检测的高效快速检测方法。通过对固相微萃取吸附剂用量、吸附时间、洗脱溶剂的优化,实现茶叶中乙酰甲胺磷的最优提取。在最优条件下,乙酰甲胺磷加标回收率可高达95%以上。本方法所使用的乙酰甲胺磷分子印记聚合物制备简单,成本低,结合效率高,易于固液分离,结合气相色谱可实现茶叶中乙酰甲胺磷的高效快速检测。     

固相微萃取技术在环境监测中的应用

固相微萃取技术(SPME)是在固相萃取技术的基础上进一步研发而来的新型分离萃取方法,以其操作简单、携带方便、费用低廉等优点在环境监测领域得到了普遍应用。本文介绍了SPME技术的基本内容、主要种类以及影响因素,并重点分析了SPME在大气环境、水体环境以及土壤环境监测中的应用,希望为行业技术发展提供一定的思考和借鉴。     

固相微萃取-气相色谱法测试凹印油墨VOC的条件优化研究

采用固相微萃取和气相色谱相结合的技术,建立了凹印油墨VOC的测试方法。通过对萃取时间、萃取温度和萃取纤维涂层膜厚等影响萃取效率的因素进行研究,获得了优化的测试条件。结果表明,气相色谱柱温箱升温程序为:50℃开始以50℃/min升至200℃,然后再以10℃/min升至230℃,保持5min;固相微萃取最佳萃取条件为:萃取时间20min,萃取温度80℃,采用100μm PDMS的萃取纤维。     

季铵盐类农药残留检测前处理研究进展

季铵盐类农药属于强碱性极性有机阳离子化合物,易残留在环境中。传统的萃取方式难以对复杂基质中的痕量残留净化富集,其前处理方法一直是检测中的难点。近年来随着固相萃取材料不断更新与发展,固相萃取法已取代液-液萃取法成为季铵盐残留检测中主要应用的前处理方法。全面地描述了各类基质中季铵盐残留检测的前处理方法,重点分析与论述了目前常用的固相萃取材料的性质及优缺点,对其在前处理分析方法中涉及的重要方面做了较全面的分析与论述。     

食用油品中己醛的分析

考察固相微萃取(SPME)以及气相色谱(GC)实验条件对食用油中己醛的检测分析的影响,实现己醛的高效萃取和分离,建立了SPME-GC-FID检测食用油中己醛的方法;对不同类实际样品的进行加标回收实验,结果表明己醛含量的回收率变化范围为85.2~110.6%,精密度为4.0~8.2%。     

分散固相萃取法测定食品中酞酸酯类物质

建立分散固相萃取-反相液相色谱法同时测定食品及模拟物中6 种痕量邻苯二甲酸酯类增塑剂(PAEs)的方法。采用正交试验分析了以HLB 为吸附材料富集净化的萃取条件,确定解析溶剂乙腈的用量为6 mL,硫酸镁为120 mg,氯化钠为120 mg。该法检测6 种样液中6 种物质峰面积对浓度进行线性回归的相关系数大于0. 999,相对标准偏差为0.3% ~4. 7% (n =5),平均回收率为62. 9% ~105. 0%,检测限为0. 019 ~0. 046 mg/ kg。该法简易、高效、成本低,具有较高回收率。     

固相微萃取技术用于牛奶中有机氯类农药残留的检测

建立了固相微萃取(SPME)-气相色谱-串联质谱(GC-MS/MS)同时测定牛奶中16种有机氯类农药残留的方法。对萃取模式、纤维涂层、萃取温度等实验条件进行了优化。用HP-5 MS弹性石英毛细管柱经柱程序升温技术分离,并用质谱检测器检测,外标法计算含量。待测农药的标准加入回收率在80%～110%之间,方法的相对标准偏差(RSD)≤9.6%,各农药组分的检出限为0.003μg/kg～0.15μg/kg。所测样品不含几种有机氯农药残留。本法简便、干扰小、检测效果好,可用于牛奶中有机氯类农药残留的检测。     

A systematic approach to optimize solid-phase microextraction. Determination of pesticides in ethanol/water mixtures used as food simulants

The optimization of solid-phase microextraction (SPME) of several organochlorine and organophosphorus pesticides is presented, and the influence of variables is discussed. The optimized method is applied to several selected ethanol/water mixtures used as food simulants, and the influence of the ethanol content on the SPME performance is also discussed. Detection limits ranging from 0.02 to 0.04 ng/g for water simulant and from 38.7 to 205.5 ng/g for 95% ethanol simulant were obtained. The relative standard deviation (% RSD) was <20% in all cases. The optimized method is compared with classical liquid-liquid extraction (LLE).     

食品罐内涂膜中有害化学物质的迁移与检测

食品罐内涂膜中有害化学物质主要有双酚A、双酚A二缩水甘油醚、双酚F、双酚F二缩水甘油醚、酚醛清漆甘油醚及其衍生物等,国际上对这些有害化学物质的使用做出了相关限定。常用的食品罐检测前处理方法有液-液萃取法、固相萃取法以及固相微萃取法等,食品罐内涂膜中有害化学物质的检测方法主要有高效液相色谱法、气相色谱-质谱法和酶联免疫法。针对食品罐内涂膜有害物质迁移的研究还存在有害物质毒性机理不健全和检测方法不完善等问题,寻找一种精确、简便且可同时检测多种有害物质的方法,并加强对有害化学物质迁移模型的建立是该领域的研究方向。     

Application of single drop microextraction for analysis of chemical warfare agents and related compounds in water by gas chromatography/mass spectrometry

Retrospective detection and identification of chemical warfare agents (CWAs) is important from the verification point of view of the Chemical Weapons Convention. In the present work, a novel method for determination of CWAs and their markers in water has been described. It is based on a single drop micro extraction (SDME) of analytes and gas chromatography/mass spectrometric identification. Extraction conditions, such as solvent selection, agitation, extraction time, and salt content, were found to have significant influence on SDME. The conditions optimized for extraction of CWAs were 1 microL CH2Cl2/CCl4 (3:1 v/v), 30-min extraction time, 300-rpm stirring rate, and with or without NaCl addition. Under optimized conditions, comparison of SDME, solid-phase microextraction, and liquid-liquid extraction was also made. The limit of detection by SDME ranged from 75 to 10 microg L(-1) at a signal-to-noise ratio of 10:1.     

Application of ceramic carbon materials for solid-phase extraction of organic compounds

Ceramic carbon materials were developed as new sorbents for solid-phase extraction of organic compounds using chlorpromazine as a representative. The macroporosity and heterogeneity of ceramic carbon materials allow extracting a large amount of chlorpromazine over a short time. Thus, the highly sensitive and selective determination of chlorpromazine in urine sample was achieved by differential pulse voltammograms after only 1-min extraction. The total analysis time was less than 3 min. In comparison with other electrochemical and electrochemiluminescent methods following 1-min extraction, the proposed method improved sensitivity by about 2 and 1 order of magnitude, respectively. The fast extraction, diversity, and conductivity of ceramic carbon materials make them promising sorbents for various solid-phase extractions, such as solid-phase microextraction, thin-film microextraction, and electrochemically controlled solid-phase extraction. The preliminary applications of ceramic carbon materials in chromatography were also studied.     

尿液中硝基安定、氯硝基安定和氟硝基安定的SepPak HPLC分析

本文介绍了一种用SepPak固相萃取技术和HPLC同时检验尿液中的苯并二氮草类药物硝基安定、氯硝基安定和氟硝基安定的方法。使用的反相色谱柱为YMC A—303C_(18)柱,以乙腈—0.01M醋酸铵(45:55,V/V)为流动相,紫外检测波长为254nm。各药物的回收率均大于80％;日内和日间测定的变异系数为1—5％。     

有机磷农药残留前处理技术的研究

本实验主要是利用固相萃取技术对食品中有机磷农药前处理方法进行了研究。对自制的固相萃取小柱的选择参数进行了优化,建立合适的样品提取、净化、浓缩的前处理方法,确保色谱分析测定时无样品基质的干扰,从而为测定的结果提供了保证,并延长色谱柱的寿命,降低了实验成本。茶叶样品以丙酮为提取剂,超声波30 min后,经florisil柱(1000mg)+活性炭(50mg)混合柱浓缩净化,用10 mL的乙酸乙酯淋洗后,经色谱分析验证,所得回收率在73.7%以上,RSD在4.1%以下,结果令人满意。     

Microwave-assisted steam distillation for simple determination of polychlorinated biphenyls and organochlorine pesticides in sediments

A novel sample extraction technique for polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) analysis using microwave-heating device is developed. In this study, microwave-assisted extraction (MAE) and steam distillation techniques were combined. Desorption of the anatytes from solid matrixes was accelerated with water vapor which was generated by microwave irradiation. A sample holder in a commercial microwave extraction cell kept the sample from direct contact with the organic solvent for analytes trapping during the treatment process. Therefore, relatively clean extracts were obtained with small amount of solvents. Without any cleanup steps, the obtained extract could be analyzed with gas chromatograph/mass spectrometers (GC/MS). Six PCB congeners (PCB15, 28, 70, 101, 180, 194, 209) and three OCPs (gamma-HCH, 4,4'-DDE, 4,4'-DDD) in two marine sediment samples (a sediment collected from a bay of Kyusyu Island, Japan, and a certified reference material NIST SRM1944) were analyzed by using this microwave-assisted steam distillation (MASD) technique and another extraction method (exhaustive steam distillation, MAE, and Soxhlet extraction); and comparisons of the results are shown in this report. Although recovery yields of highly chlorinated biphenyls (PCB180, 194, 209) and relatively polar OCPs (gamma-HCH, 4,4'-DDD) were low (30-60%) compared with other analytes (PCB15, 28, 70, 101, 4,4'-DDE; recovery, 80-100%), use of isotope labeled internal standards for the MASD technique gave comparable results with the values obtained by other extraction methods and the certified values in the samples.     

液-液小体积萃取GC-MS方法快速测定地表水中的硝基苯类、氯苯类及邻苯二甲酸酯类化合物

建立了一种以容量瓶为萃取容器的液-液小体积萃取GC-MS快速测定地表水中硝基苯类、氯苯类及邻苯二甲酸酯类化合物的分析方法。该方法具有操作简单快速、适用性广和试剂用量很少等特点。当萃取试剂用量为1mL时(约为一般常规液液萃取用量的数十分之一),萃取富集效率可达100倍,回收率为76%～120%,相对标准偏差为3%～8%,检出限为0.2～0.9μg/L。对实际地表水水样中的硝基苯、氯苯类及邻苯二甲酸酯化合物进行了定性定量分析,结果令人满意。