高效液相色谱串联质谱法直接测定环境水样中8种有机磷农药

建立了一种高效液相色谱-串联质谱法（LC-MS/MS）同时测定环境水样中8种有机磷农药的分析方法。以地表水、地下水、污水和废水样品作为代表性水样基底,前处理方法仅采用简单的滤膜过滤,在C₁₈柱分离后,在多反应监测模式下进行分析检测。结果表明,敌百虫、毒死蜱等有机磷农药在样品保存过程中迅速发生降解,分析须在样本采集后1 d内完成;该方法的检出限为0.10~0.20 μg/L,线性拟合相关系数（r）均>0.995;不同基底、不同浓度的加标回收实验表明,8种有机磷农药在环境基底中的回收率为74.5%~118%,相对标准偏差为0.4%~8.6%。该方法操作简便、灵敏度高、准确性好,在未来环境监测工作中具有较好的应用前景。     

利用MALDI-TOF MS技术简便、快速检测水华蓝藻的方法研究

以水华蓝藻为研究对象,用基质辅助激光解吸电离飞行时间质谱(MALDI-TOF MS)技术对其进行测定分析并获得了蛋白质指纹图谱。对铜绿微囊藻标准株(NIES-843)样品通过3种前处理方法得到的质谱图进行对比,确定了质谱分析的样品前处理方法,建立了利用MALDI-TOF MS技术简便、快速检测水华蓝藻的方法。对在水华中出现的4种不同蓝藻进行MALDI-TOF MS分析,结果表明各种蓝藻具有其特征性波谱,可据此对水华蓝藻进行区分和鉴定。该方法快速、简便、精确、可程序化,具有广泛的应用前景。     

GC/MS法测定生物样品中多溴联苯醚类化合物

本研究建立了多溴联苯醚（PBDEs）生物样品分析方法,获得了优化的前处理条件、气相色谱和质谱检测条件.对定性定量方法及实验条件必须满足的要求进行了评价.通过质量控制（quality control, QC）对整个方法进行了验证.结果证明,本研究所建立的分析方法满足生物样品PBDEs测定的要求,回收率在50.5%～112.3%之间,回收率相对标准偏差在5.3%～9.9%之间,方法检测限在7.1～161.8 pg/g之间.在建立的方法基础上,测定了部分养殖和野生鱼类样品,测得的野生鳜鱼和鲫鱼以及2个养殖鲈鱼样品的结果分别为1.53、1.11、5.31和6.15 ng/g(干重),其中主要的同族体为BDE47.     

Identification and characterization of Fe3O4/peroxodisulfate advanced oxidation products from sulfameter

Sulfonamides (SAs) are one of the most widely used antibiotics and their residuals in the environment could cause some negative environmental issues. Advanced oxidation such as Fenton-like reaction has been widely applied in the treatment of SAs polluted water. Degradation rates of 95%-99.7% were achieved in this work for the tested 8 SAs, including sulfisomidine, sulfameter (SME), phthalylsulfathiazole, sulfamethoxypyridazine, sulfamonomethoxine, sulfisoxazole, sulfachloropyridazine, and sulfadimethoxine, in the Fe₃O₄/peroxodisulfate (PDS) oxidation system after the optimization of PDS concentration and pH. Meanwhile, it was found that a lot of unknown oxidation products were formed, which brought up the uncertainty of health risks to the environment, and the identification of these unknown products was critical. Therefore, SME was selected as the model compound, from which the oxidation products were never elucidated, to identify these intermediates/products. With liquid chromatography-high resolution tandem mass spectrometry (LC-HRMS/MS), 10 new products were identified, in which 2-amino-5-methoxypyrimidine (AMP) was confirmed by its standard. The investigation of the oxidation process of SME indicated that most of the products were not stable and the degradation pathways were very complicated as multiple reactions, such as oxidation of the amino group, SO₂ extrusion, and potential cross-reaction occurred simultaneously. Though most of the products were not verified due to the lack of standards, our results could be helpful in the evaluation of the treatment performance of SAs containing wastewater.     

2,3,7,8-TCDD代谢产物的液-质联用分析

采用肝微粒体体外温孵法,对2,3,7,8-TCDD在大鼠肝微粒体中进行体外代谢研究.利用实验中所建立的液相色谱串联质谱方法对其代谢产物进行直接分析,共鉴别出两类代谢产物,分别为2个单羟基化代谢产物(2-OH-1,3,7,8-TCDD和1-OH-2,3,7,8-TCDD)和双羟基化脱氯的代谢产物.     

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.     

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.     

气相色谱—串联质谱法检测水中苯霜灵、甲霜灵、噁霜灵残留量

建立水中甲霜灵、苯霜灵、噁霜灵农药残留量的气相色谱—串联质谱(GC-MS/MS)的检测分析方法。样品采用乙腈提取、固相萃取(SPE)柱净化。采用GC-MS/MS分析时,三种农药在15 mim内完全分离并流出。添加浓度加标回收率为80.6%~88.4%,相对标准偏差(RSD)小于5.0%。在0.01~0.20 mg/L质量浓度范围之间线性关系良好(r~20.999 0)。该方法的灵敏度、精密度和准确度均满足农药残留分析要求,适用于水中的农药残留的快速筛查与定性、定量分析。     

气相色谱-质谱法测定沉积物中的有机氯和多氯联苯

采用加速溶剂萃取法提取沉积物中的有机氯和多氯联苯,提取液用凝胶色谱法净化后用气相色谱-质谱法测定。方法在5.00μg/L~200μg/L范围内线性良好,当取样量为10.0 g时,方法检出限为0.03μg/kg~0.37μg/kg,空白样品2个质量比水平的加标回收率为70.8%~121%,测定结果的RSD为2.7%~11.5%。用该方法测定实际样品,结果 12个抽检的沉积物样品中多氯联苯均未检出,9个样品中有机氯检出。     

大气VOCs在线监测系统测量准确性分析

基于在线气相色谱-氢火焰离子检测/质谱(GC-FID/MS)方法,在线测量116种大气挥发性有机物的性能指标(线性关系、检出限、精密度、正确度、期间正确度和期间精密度).基于在线监测系统连续7d的实际运行情况,定量评估116种有机物在实际长期运行中测量的准确性和可靠性.结果 表明,116种组分中,109种组分的线性相关...