β-蒎烯的液相臭氧化反应研究

研究β－蒎烯的液相臭氧化反应,利用ＧＣ／ＭＳ联用系统监测,分析了反应的全过程,确定臭氧化反应的主要产物是不蒎酮,产率为４６％,在Ｏ３存在下稳定,无次级反应,根据液相反应的分析结果,对气相反应的可能机理进行了讨论。     

北京大气中BTEX的观测分析与研究

采用二步深冷浓缩与气相色谱/质谱联机对北京大气中的苯类物质(BTEX) 进行了长期连续观测.最近4年观测数据表明:日变化有双峰和3峰变化,冬、春季呈现与交通高峰期吻合的双峰变化,即上午08:00至10:00和下午17:00前后各出现一个高值;秋季日变化中,夜间22:00出现第3峰值;夏季日变化呈3峰型,最大峰值在正午前后.2000～2002年BTEX月平均总浓度为(44.1±24.5) nmol/mol(碳单位),季变化峰值出现在夏季.年际变化趋势中,北京大气BTEX的总平均浓度从 1999 年到2002年大幅度下降.     

泥沙对双酚A的吸附及其影响因素研究

以黄河泥沙为例,用SPE HPLC MS MS的方法分析了双酚A在泥沙上的吸附规律及其影响因素.结果表明,由于黄河泥沙碳酸盐含量较高,双酚A的等温吸附规律不能用线性吸附方程和Freundlich吸附方程来描述;去除泥沙中碳酸盐后,泥沙对双酚A的吸附量增加,且其吸附规律可用线性吸附方程和Freundlich吸附方程来描述.泥沙总有机质含量和可溶态有机质含量都会影响双酚A的吸附,沉积物和悬浮物对双酚A的吸附量分别与其可溶态有机质含量负相关;由于价态不同,钙离子和钾离子对双酚A的吸附影响规律相反,随着钙离子浓度的增加双酚A吸附量亦增加,而随着钾离子浓度的增加双酚A吸附量却减少.     

洹河底泥中有机污染物调查与分析

介绍了GC/MS联用仪对河流底泥中微量有机污染物进行定性、定量分析的实验方法,探讨了底泥与地表水中有机物种类和含量间的关系。     

制药废水中头孢类抗生素残留检测方法及环境风险评估

基于固相萃取-超高效液相色谱-两级串联质谱(SPE-UPLC/MS/MS)技术,建立了制药废水中头孢克洛、头孢曲松、头孢氨苄、头孢噻肟、头孢唑啉、头孢呋辛、头孢西丁、头孢噻吩和头孢拉定共9种头孢类抗生素的测试方法,定量限为27.5~131.8ng/L,目标物回收率为72.8%~102.2%;利用该技术,检测某采用两级生物氧化工艺的制药废水处理厂各级单元出水,共检测出头孢曲松、头孢唑啉、头孢噻肟和头孢呋辛4种头孢类抗生素,其在进水中平均浓度分别为7.6,12.9,5.6,91.6μg/L,在一级氧化出水中平均浓度分别为4.2,5.2,2.2,37.4μg/L,在二级氧化出水中平均浓度分别为2.0,2.7,0.6,24.4μg/L;风险商值法评估制药废水出水中残留的头孢曲松、头孢唑啉、头孢噻肟和头孢呋辛的环境风险均为高风险等级.     

亲水荷电超滤膜的制备及对腐殖酸的分离性能

为改善聚醚砜(PES)超滤膜的抗污染性能和提高对腐殖酸(HA)的截留率,以介孔二氧化硅(MS)为添加剂,采用相转化法制备了亲水性PES/MS复合超滤膜,并对膜表面进行荷电改性.研究了MS对膜的断面结构、表面化学性质和过滤性能的影响,考察了荷电改性PES/MS超滤膜对水中HA的分离性能以及溶液pH值、离子强度和钙离子浓度等因素对荷电膜超滤过程的影响.SEM表征结果显示,MS颗粒在PES/MS复合膜的表面分散均匀,膜孔的连通性改善.亲水荷电改性后,膜表面接触角由68°降至57°,zeta电位由-6.31mV降至-11.45mV,膜对HA的去除率由72%提高到95%,通量衰减率由29.8%减小到4.9%.结果表明,对PES超滤膜进行亲水荷电改性可有效提高对HA的截留率,同时减轻膜污染;另外,溶液的pH值、离子强度和钙离子浓度对荷电超滤膜的过滤性能有较大影响,调节合适的溶液环境可在提高截留率的同时,减轻膜污染.     

超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法同时测定污水中14种有机磷酸酯阻燃剂(OPEs)的分析方法.样品采集后,经GF/C膜过滤,HLB固相萃取小柱净化后进样分析.以BEH C18色谱柱为分离柱,乙腈和水混合液为流动相(0.2 mL min-1)梯度洗脱,15 min内可完成14种OPEs的分离.在电喷雾正离子模式下,采用多反应监测模式(MRM)进行质谱测定.在加标浓度为1.0μg·L-1时,14种OPEs在污水处理厂进水和出水中的回收率分别为52.1%—119%、43.6%—114%,相对标准偏差(RSD)分别为1.2%—16.2%、0.4%—9.2%,方法的检出限(LOD)在0.3—6.0 ng·L-1间.方法精密度好,准确度高,可满足同时对污水样品中的14种OPEs进行定性及定量分析的要求.     

工业废水对洹河有机污染的调查与分析

采用适当的样品前处理技术,利用GC/MS对洹河水及焦化厂、染料厂废水进行有机污染物的分析,确定了工业废水对洹河造成有机污染的主要化合物,从而为企业污水的处理和洹河治理提供依据.     

Standard purity and response factors of perfluorinated compounds

It has been reported that the relative response factors of isotopically labeled standards and unlabeled standards of the same perfluorinated compounds could be different. Individual (100 ng mL^?1) solutions of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) were analyzed using high-performance liquid chromatography tandem mass-spectrometry under negative-ion electrospray to detect any impurities present down to 0.5%–0.1% relative to the major component. Purity of the standards ranged from approximately 86% to ≥ 97%. Standard solutions of unlabeled and isotopically labeled materials were analyzed to compare the response factors of isotopically labeled analytes versus their nonlabeled counterparts in three different matrices at equivalent concentrations: organic solvent (methanol), serum extract, and water present individually and concurrently. Not all labeled analytes have the same response factor as their nonlabeled complement, and in at least one case the matrix in which the standard is present may cause significant suppression of response. Standard solutions of electrochemical fluorination produced PFOA and PFOS were quantified under multiple reaction monitoring mode, using calibration curves prepared from standards consisting primarily of linear standards only. The use of linear only standards may cause under-prediction of concentrations, and that the working range of these standards may be limited.     

Evaluation of pesticides multiresidue contamination of khat leaves from Jazan region,Kingdome Saudi Arabia,using solid-phase extraction – gas chromatography/mass spectrometry

The habit of khat chewing is widespread with a deep-rooted sociocultural tradition in these regions and as such poses a public health problem. The use of pesticides is considered to be indispensable practice for the production of adequate food supply for the increasing demands by the global population and for control of insect-borne diseases. Thus, contamination of the environment with pesticides and entry of these chemicals into the food chain is unavoidable especially in developing countries. The main objective of our current study was to assess pesticide pollution of khat leaves (unknown origin) obtained while being smuggled into the Kingdom of Saudi Arabia and to be used in Jazan area. A total of 120 khat leaf samples were extracted using solid-phase extraction followed by gas chromatography/mass spectrometry analysis for the presence of 69 standard pesticides using an internal standard, tiphenyl phosphate. No pesticide residues were detected in all the studied samples. These data as preliminary and more experiments need to be performed to confirm our present findings. Routine monitoring of the pesticide residues is important for the prevention, control, and reduction of environmental pollution and also for legal decisions to minimize health risks.