气相色谱/质谱联用法测定环境空气中恶臭类硫化物

采用冷阱预浓缩-气相色谱/质谱联用法测定环境空气中硫化氢、甲硫醇、甲硫醚、二硫化碳、二甲二硫、噻吩等6种硫化物,讨论了采样容器材质的影响。方法线性良好,6种硫化物的检出限为1.0μg/m3～5.0μg/m3,混合标准气平行测定的RSD≤8.1%,加标回收率为93.5%～97.3%。     

SBSE-GC/MS法测定饮用水源水中7种多氯联苯单体

采用搅拌棒吸收萃取(SBSE)-溶剂解吸-气相色谱/质谱联用法测定饮用水源水中7种多氯联苯单体,优化了萃取和解吸条件。方法在5 ng/L~100 ng/L范围内线性良好(r≥0.979),7种多氯联苯单体的检出限为0.8 ng/L~3.4 ng/L(100 mL水样SBSE萃取2 h),加标10 ng/L时实际水样回收率为93.0%~116%。     

液液萃取-气相色谱-质谱法同时测定饮用水中的酞酸酯、百菌清和联苯胺

建立了液液萃取-气相色谱-质谱（LLE -GC/MS）同时测定饮用水中的6种酞酸酯类化合物、百菌清和联苯胺的方法。选用3种有机溶剂进行萃取,筛选出回收率高、操作简单的前处理方法,萃取后经气相色谱-质谱分析。方法表明：8种物质线性良好,相关系数为0．9978～0．9995,用二氯甲烷萃取回收率最佳,回收率在90．1％～118％之间,相对标准偏差在0．24％～7．21％之间。     

基体改进剂在电感耦合等离子体质谱分析中的应用

基体改进剂在电感耦合等离子体质谱仪(ICP-MS)中的应用引起了人们很大的关注,对近年来化学改进剂在ICP-MS中的应用进展作了介绍,对各种改进剂的改进效果及机理进行阐述。     

P&T-GC-MS法测定水中54种挥发性有机物

建立了同时测定水中54种挥发性有机物(VOCs)的吹扫捕集-气相色谱-质谱联用法,并对吹扫捕集条件进行了优化。优化后的方法,54种VOCs在0.50~40.00μg/L质量浓度范围内线性良好,相关系数R2均0.995 6,检出限为0.021~0.105μg/L,加标回收率为76.4%~110.8%,相对标准偏差为2.33%~15.8%。该法操作简单,消耗费用低,分析速度快,具有良好的灵敏度、回收率和重现性,能够满足生活饮用水中54种VOCs的同时测定。     

SPE-GC-MS/MS法测定水源水中多种有机氯EDCs

采用C 18柱固相萃取(SPE)-三重四级杆气相色谱-质谱法同时测定水中18种含有机氯的环境内分泌干扰物,方法在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.04 ng/L^0.8 ng/L,空白水样的加标回收率为61.3%~108%,6次测定结果的RSD为3.8%~18.0%。将该方法用于饮用水源水监测,18种目标化合物的测定值为未检出~1.5 ng/L,平均加标回收率为71.9%~109%,平行测定结果的RSD<15%。     

气相色谱/质谱法测定水中15种酞酸酯类化合物

采用固相萃取-气相色谱/质谱法测定水中15种酞酸酯类化合物,确定方法的最优条件为:依次用10 m L正己烷和丙酮混合溶剂(V/V=5∶1)、甲醇和空白试剂水活化C18固相萃取柱后,水样以5 m L/min过柱萃取,再以8 m L正己烷:丙酮(V/V=5∶1)混合溶剂洗脱后,浓缩至1 m L,进气相色谱/质谱测定。该法的检出限为0.18~0.38μg/L,在0.50~20.0 mg/L范围内线性良好,相关系数均0.996。空白水样的加标回收率为71.8%~120%,相对标准偏差为1.73%~12.7%;实际废水水样的加标回收率为64.8%~135%,相对标准偏差为2.75%~18.0%。     

热脱附-GC/MS法测定垃圾填埋场周围空气中氯代烃

采用热脱附-冷阱捕集-GC/MS法测定垃圾填埋场周围空气中24种氯代烃,通过试验优化并确定热脱附质谱的最佳处理条件。方法在5.00 mg/L～100 mg/L范围内线性良好,24种氯代烃的方法检出限为0.060μg/m~3～0.200μg/m~3,测定下限为0.240μg/m~3～0.800μg/m~3。空白加标回收率为91.8%～110%,6次测定结果的RSD均5%。实际样品测定结果为0.112 mg/m~3～0.412 mg/m~3,表明离垃圾填埋场最近的居民区环境中氯代烃为未检出或痕量分布,对生命体危害极低。     

Emission and burnt smell characteristics from combustion experiments with defined materials

Typical burnt smell often results from fire accidents or in general from incomplete combustion. Recently, eleven compounds were identified, which are basically responsible for this odour. When analyzing residual materials from different fire accidents, the pattern that means the relative ratios of these compounds among each other varies strongly, although always causing a burnt smelling. Consequently, lab-scale combustion experiments were performed in order to investigate the influence of defined materials from domestic environment on the burnt-smell fingerprints. Furthermore, the occurrence of other polar and higher molecular combustion products was studied. It was found that under good combustion conditions, the burnt smell patterns resulting from the single materials were astonishingly consistent, mostly dominated by methylphenols or naphthalene. No correlation could be found between these ‘fingerprints’ and combustion product groups identified by GC/MS-screenings. LC/MS/MS-measurements especially pointed at the existence of higher molecular weight phenolic and acidic functionalized compounds in the combustion residues.     

Simple analytical method for determination of pesticide residues in human serum by liquid chromatography tandem mass spectrometry

The aim of this study was to develop an analytical method for the determination of residues of organophosphorus and carbamate pesticides which are widely used in Tunisia. This method involves a liquid-liquid extraction procedure followed by liquid chromatography tandem mass spectrometry (LC/MS/MS) for the identification and quantification of compounds. Ionization of molecules was performed by the electrospray mode. Multiple reactions monitoring (MRM) was the acquisition mode used for the monitoring of two MS/MS transitions for each compound. The average recoveries obtained, at three different fortification levels, ranged between 65% and 106% for most of the pesticides studied, except for methamidophos (lower than 25%).The linearity of the method was in the range of 5 to 50 μ g/L with a correlation coefficient from 0.995 to 0.999, depending on the analyte. The estimated limit of detection and limit of quantification were 2 μ g/L and 5 μ g/L, respectively. The precision of the analytical procedure was satisfactory and the coefficients of variation, evaluated at three concentration levels were lower than 15% for most pesticides studied. The application of the method was investigated in a population of agricultural workers chronically exposed to various pesticides some of which, such as carbofuran, carbendazim, methomyl and pirimicarb, were detected in some serum samples.