HPLC-MS/MS法同时测定近岸底栖生物中15种磺胺类抗生素残留量

采用液-液萃取和固相萃取方法处理生物样品,建立以ESI(+)和SRM为基础的快速检测15种磺胺的HPLC-MS/MS方法,并采用该方法对大连周边海域底栖生物中磺胺的残留状况进行了分析. 结果表明:近岸底栖生物中磺胺噻唑(STZ)、磺胺喹啉(SQX)、磺胺嘧啶(SDZ)和磺胺甲基异唑(SMZ)等检出率较高,质量分数为1.39～143.29 ng/g.说明在我国近岸底栖生物中已经有一定量的磺胺类抗生素的残留,并威胁到水生生物的安全,因此应加强对近岸海洋环境中抗生素残留的监测与管理.      

HPLC-MS/MS高通量检测动物源食品中的β-肾上腺素兴奋剂

本文建立了用LC/MS/MS定量分析19种β-肾上腺素兴奋剂的方法,讨论了不同液相色谱方法对灵敏度的影响,结果是小流速的分离度好,但分析时间长,大流速分离度一般,但分析时间可节省很多,对定量检测的灵敏度影响很小.     

2007年夏季北京大气CO检测分析

采用经过改进的装配有氧火焰离子化检测器(FID)的气相色谱仪(GC),配合自动进样、分析和标定系统,以10min一次的采样频率,于2007年7月-9月,在中国科学院大气物理研究所铁塔分部连续采样,监测北京大气CO浓度变化.结果表明,北京城市大气CO浓度日变化呈双峰型,两峰值出现的时间分别为7:00-8:00和23:00-24:00,浓度分别达3.66×10-6V/V和4.92×10-6V/V.北京大气CO的浓度变化受源排放强度和气象要素共同影响.机动车限行,对降低大气CO的浓度效果明显,但天气过程对CO的清除作用也不可忽视.     

环境水中全氟羧酸及全氟磺酸类化合物(PFCs)的分析

本文采用Agilent 641O LC/MS/MS液相色谱-三重串联四极杆质谱建立了水中全氟辛酸(PFOA)、全氟壬酸(PFNA)、全氟癸酸(PFDA)、全氟辛烷磺酸(PFOS)、全氟十二烷酸(PFDoA)等五种全氟羧酸及磺酸类化合物在环境水中残留基测定的高效液相色谱-串联质谱方法,样品前处理采用Agilent SampliQ OPT固相萃取小柱进行浓缩净化,回收率＞50%,五种化合物的线性均大于0.997,对环境水样品的检测灵敏度可达0.2 pg·ml-1.     

北京市工业废水和城市污水中有机氮、有机磷类农药残留分析

建立了基于^18C固相萃取柱和气相色谱／氮磷检测器(GC／NPD)分析水体中环境激素类物质——有机氮、有机磷类农药的分析方法．并对方法的回收率、灵敏度进行了评价。同时分析了北京市七类典型污染点源50个采样点位有机氮、有机磷类农药的浓度。检出的有机氮、有机磷农药包括马拉硫磷、莠去津、对硫磷和乙草胺．检出率都较低。低于8％;检出有机氮、有机磷农药的浓度范围是0．11～4．02mg／L。该方法对有机氮、有机磷农药的回收率除嗪草酮为30％外．其余在83．9％～94．7％之间。     

Pyrolysis behaviors of oil sludge based on TG/FTIR and PY-GC/MS

Pyrolysis is an alternative technology for oil sludge treatment. Thermogravimetric Analysis-Fourier Transform Infrared Spectroscopy and Pyrolysis-Gas Chromatography/Mass Spectrometry were employed to investigate the pyrolysis process and products of oil sludge. The pyrolysis process was divided into five stages: drying and gas desorption, oil volatilization, main pyrolysis, semi-coke charring, and mineral decomposition. The main reaction temperatures ranged from 497.6 K to 753.2 K. The products were mainly composed of pairs of alkane and alkene (carbon number ranges from 1 to 27). The mechanisms consisted of random chain scission followed by end chain scission at high temperatures with volatilization occurring during the whole process. This study is useful not only for the proper design of a pyrolysis system, but also for improving the utilization of liquid oil products.     

顶空-固相微卒取-气相色谱测定水体中痕量苯系物

对测定水体中痕量苯系物的顶空-固相微萃取-气相色谱法的固相微萃取条件进行了对比优化,经过对水体中的7种苯系物对比实验,确定了顶空-固相微萃取-气相色谱法的固相微萃取的最佳实验条件为：选用75μmCAR/PDMS萃取涂层,加入与水质量比为40%的氯化钠,于20℃温度下萃取40min,解析3min。方法检出限为0.12～0.19μg/L,相对标准偏差2.0%～3.9%。依据确定的优化条件,用不同类型的水样对优化后的试验条件进行了验证试验,回收率在96.2%～102.0%之间,表明优化后的试验条件适用于多类型水体中痕量苯系物的分析测定。     

57种臭氧前体有机物混合标准气体量值比对研究

标准物质的量值准确性是监测数据准确的重要前提。为科学评价57种臭氧前体有机物混合标准气体量值的准确性,研究建立了定量环进样-中心切割-气相色谱-双火焰离子化检测器分析方法与量值比对方法(E_n值法),并对市售6个品牌各2个批次标准气体开展量值比对研究。研究结果表明,4个品牌标气量值一致性、准确性较好,2个品牌存在5～22种组分量值偏离(E_n绝对值为1.0～5.3),用于开展臭氧前体有机物监测的标准物质质量仍需持续监督、提升。     

Ultra trace simultaneous determination of 50 polycyclic aromatic hydrocarbons in biota using pMRM GC-MS/MS

Abstract

A saponification extraction method with gas chromatography pseudo-MRM (pMRM) mass spectrometry detection was developed for the determination of 50 total polycyclic aromatic hydrocarbons (TPAH50, a combination of parent and alkylated homologues) in biota. The method was aimed at monitoring and identification of potential TPAH contaminants in bitumen impacted environments. Alkylated PAHs were determined by multi-level, quantitative calibration using parent PAHs. The developed and thoroughly validated method required only one injection for TPAH50 analysis which represents significant saving of time and expensive authentic alkylated standards. The current method was tested with certified reference mussel tissue NIST 1974c and performed well. In a comparison study, the method reached a limit of quantitation (LOQ) for the TPAH50 between 0.1 and 0.2?ng g^?1, while the QuEChERs enhanced matrix removal – lipid (EMR) kit produced by Agilent showed an LOQ of 5–10?ng g^?1. The current method relied on response factors (RF) for the quantitation of alkylated PAHs determined against parent PAHs. These RFs were shown to be stable and consistent over the course of 1 year, during which over 200 routine environmental biota monitoring samples were analyzed. The environmental biota monitoring samples analyzed include muscle, carcass and liver, with an average total PAH50 concentration of 13, 90 and 135?ng g^?1, respectively. Results show significant differences in the distributions of 1 ringed, 2 ringed, 3 ringed, 4 ringed, and 5+ ringed TPAHs between the types of biota samples.     

绿证交易、发售电配额制与可再生能源财税减负效应

为促进清洁能源消纳利用和减轻标杆电价政策财税负担,绿色电力证书(绿证)核发和认购制度已在全国试行。为验证两类政策并存下绿证交易的财税减负作用,该文构建绿证定价和财税减负效应模型,分类探讨不同交易机制和配额安排:绿证自由市场、发售电配额强制市场交易如何影响售证方定价策略和配额主体履约抉择,论证绿证市场均衡和政策互动如何影响可再生能源补助支出、电价附加和绿证交易的税负转嫁效应。模型论证与分类市场情景表明:①绿证交易提供了低成本履约的制度安排,有助于财税减负;②电力市场管制和交叉补贴电价政策下,发电商配额导致火电企业最优履约抉择是自建绿电项目而非绿证交易,绿证市场有价无市;③售电配额的市场交易效率更高,但发电商实施领导跟随-产量最优策略将造成电力和绿证价格双攀升,变相增加电价负担;④并网消纳和补贴拖欠削弱绿证价格而降低补贴转嫁,售电配额调整通过跨区绿电需求变化影响税负转嫁。这些结论蕴含的政策意义是:①兼顾绿电支付意愿、成本分担与应用目标,健全绿证认购市场体系;②理顺绿证定价与惩罚机制,确保绿证市场竞争均衡与履约效率;③完善省级配额机制,引导具备成本优势的跨区绿证交易;④协调政策互动效应,增强绿电溢价和绿证减负效应。