气相色谱质谱法测定纺织品中N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和N-甲基吡咯烷酮溶剂残留

建立了气相色谱质谱法测定纺织品中N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAC)和N-甲基吡咯烷酮(NMP)的方法.纺织品中N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和N-甲基吡咯烷酮经丙酮超声萃取,用0.45μm滤膜过滤后直接进样,将提取物进行GC-MS定性定量分析.结果表明,在0.1—10μg·mL-1线性范围内,DMF、DMAC和NMP线性方程分别是y=75041x+8039,y=71622x+12371,y=96278x+8548,相关系数均大于0.9995;方法检出限DMF和DMAC为5 mg·kg-1,NMP为3 mg·kg-1;平均回收率为86.3%—92.0%;相对标准偏差(n=6)为1.4%—5.0%.该方法简便、快速、灵敏度高、重复性好,可用于测定纺织品中N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和N-甲基吡咯烷酮.     

液相色谱-串联质谱法检测猪肉中肾上腺素及其代谢物残留

针对猪肉中新兴的肾上腺素及其代谢物3,4-二羟基扁桃酸、4-羟基-3-甲氧基-扁桃酸,基于"肾上腺素作用翻转"机理同步添加的异丙嗪,建立了超高效液相色谱-串联质谱检测方法.4种物质线性良好,相关系数均大于0.999;猪肉基质的定量限(LOQ, S/N=10)依次为25、100、5、0.1μg·kg~(-1),精密度(RSD)均小于10%,平均回收率在78.3%—92.5%.     

气相动态顶空法分析水源水中61种挥发性有机物

建立了用于饮用水源水中61种挥发性有机物（VOCs）同时进行分析的气相-动态顶空进样-气相色谱-质谱法（D-HS-GC-MS）,VOCs包括集中式生活饮用水地表水源地特定项目中的31种VOCs。用D-HS-GC-MS法对水样中VOCs进行分析,获得良好的标准曲线线性关系（均大于0.995,溴二氯甲烷除外）,除乙醛、丙烯醛、丙烯腈和环氧氯丙烷的方法检出限分别为15 g/L、13 g/L、11 g/L和11 g/L外,其余VOCs的方法检出限均介于0.10～0.58 g/L,饮用水源水实际样品加标回收率和RSD分别为75.8%～116%和1.16%～21.6%（n=3）。气相-动态顶空进样法相对于常见的吹脱捕集法具有不直接接触样品的优势,避免了仪器被样品污染,用于饮用水源水中几十种VOCs的同时分析,在常规监测中可节省大量的人力物力投入。     

测定13种抗生素的固相萃取-高效液相色谱串联质谱法优化与应用

大量用于预防和治疗细菌和真菌性等疾病的抗生素药物未经完全代谢后最终进入自然水体,对饮用水源水质安全构成潜在威胁.为快速测定饮用水源水体中的抗生素残留,保障饮水安全,本论文建立一种固相萃取-高效液相色谱串联质谱法测定13种抗生素的分析方法.采用OASIS^? HLB小柱对水样进行固相萃取富集和净化,以甲醇和0.5%的甲酸(含5 mmol·L^-1乙酸铵)水溶液为流动相,经Kinetex^?C18色谱柱分离后采用三重四极杆串联质谱多反应监测模式分析.该方法检出限为0.05—1.66 ng·L^-1,定量限为0.17—5.52 ng·L^-1,回收率为70.2%—121.5%,相对标准偏差为1.1%—13.5%.该方法准确度高,灵敏度高,适用于饮用水源源水中痕量抗生素残留的测定.方法成功应用于厦门市饮用水源源水中抗生素残留分析,共检出7种抗生素,浓度范围为ND—32.6 ng·L^-1.     

气质联用法检测日用化学品中二甘醇

建立了气相色谱质谱联用(GC-MS)检测日化品中二甘醇含量的方法.样品先用海砂研磨,无水硫酸钠除水,再用甲醇超声提取20min,过滤后直接检测.采用外标法,选择离子定量.二甘醇在1.0～50.0mg/kg质量比范围内线性关系良好,相关系数为0.999 4.在5～20 mg/kg添加水平的平均回收率为95.2%～108.2%,相对标准偏差为2.2%～4.5%.实验表明,该方法适于日化品中二甘醇含量的检测.     

激光质谱法对机动车尾气中污染物的测量

本文详细介绍了一种全新的污染物测试方法———激光质谱法的原理和特点。我们应用这一方法对机动车尾气进行了初步探测 ,得到了 2 6 6nm激光作用下汽车尾气的激光电离质谱图 ,并对摩托车发动机运行状态与苯系列污染物排放量之间的关系进行了初步的在线测量     

顶空/气相色谱—质谱法测定固体废物中挥发性卤代烃的研究

建立了顶空,气相色谱-质谱法同时测定固体废物中35种挥发性卤代烃的方法,系统地研究了顶空条件对测定结果的影响,优化了色谱分离条件。结果表明,各挥发性卤代烃可以实现良好的分离;标准曲线相关系数均大于0．99,检出限为2-3μg/kg,不同浓度的相对标准偏差分别为5．3％～19％,1．8％-17％和4．2％-15％,样品加标回收率为70．8％-118％。该方法灵敏度高,具有良好的精密度和准确度,适用于固体废物中挥发性卤代烃的测定。     

焦炉烟气中二（口恶）英类物质排放水平研究

二噁英和类二噁英多氯联苯属于《关于持久性有机污染物的斯德哥尔摩公约》规定的非故意产生的持久性有机物,统称为二噁英类物质.焦化生产过程中具备二噁英类物质生成所需的前体物、温度、催化剂等条件,但目前国内外对焦化行业焦炉烟气二噁英类物质排放研究仍属空白,为进一步明确焦化行业排放水平和影响因素,针对性地提出行业减排和控制措施,利用高分辨气相色谱-高分辨质谱法对4个不同规模的典型焦化企业焦炉烟气中二噁英类物质排放情况进行现场采样和实验室分析.结果表明,二噁英类物质毒性当量(以WHO-TEQ计)范围为3.9~30.0 pg·m-3,处于较低水平,检出较多的PCDD/Fs同系物主要是高氯代的.另外,烟气中此类物质的排放量与焦化生产工艺关系密切,捣鼓炼焦、较高的炭化室高度有利于减少二噁英类物质的排放.     

Oxidative capacities of size-segregated haze particles in a residential area of Beijing

The frequent haze days around the Chinese capital of Beijing in recent years have aroused great attention owing to the detrimental efects on visibility and public health. To discover the potential health efects of the haze, oxidative capacities of airborne particles collected in Beijing during haze and clear days were comparably assessed by a plasmid scission assay. Eleven water-soluble trace elements(As, Cd, Cr, Cu, Mn, Ni, Pb, V, Se, Tl, and Zn) in the size-segregated airborne particles were quantitatively analyzed by inductively coupled plasma mass spectrometry, and most of the watersoluble trace elements were found to mainly concentrate in the fine particle size of 0.56–1.0 μm. In comparison with clear days, the mass concentrations of 11 analyzed water-soluble trace elements remarkably increased during haze days, and the oxidative capacities determined by the plasmid scission assay were markedly elevated accordingly during the haze days under the same dosage of particles as for those during clear days. Water-soluble trace elements in airborne particles, such as Cu, V, and particularly Zn, were found to have significantly positive correlations with the plasmid DNA damage rates. Because Cu, V, and Zn have been considered as bioavailable elements, the evident increase of these elements during haze days may be greatly harmful to human health.     

Rapid detection of multiple class pharmaceuticals in both municipal wastewater and sludge with ultra high performance liquid chromatography tandem mass spectrometry

This work described the development, optimization and validation of an analytical method for rapid detection of multiple-class pharmaceuticals in both municipal wastewater and sludge samples based on ultrasonic solvent extraction, solid-phase extraction, and ultra high performance liquid chromatography-tandem mass spectrometry quantification. The results indicated that the developed method could effectively extract all the target pharmaceuticals （25） in a single process and analyze them within 24 min. The recoveries of the target pharmaceuticals were in the range of 69%-131% for wastewater and 54%-130% for sludge at different spiked concentration levels. The method quantification limits in wastewater and sludge ranged from 0.02 to 0.73 ng/L and from 0.02 to 1.00μg/kg, respectively. Subsequently, this method was validated and applied for residual pharma- ceutical analysis in a wastewater treatment plant located in Beijing, China. All the target pharmaceuticals were detected in the influent samples with concentrations varying from 0.09 ng/L （tiamulin） to 15.24 μg/L （caffeine）; meanwhile, up to 23 pharmaceuticals were detected in sludge samples with concentrations varying from 60 ng/kg （sulfamethizole） to 8.55 mg/kg （ofloxacin）. The developed method demonstrated its selectivity, sensitivity, and reliability for detecting multiple-class pharmaceuticals in complex matrices such as municipal wastewater and sludge.