加速溶剂萃取-气相色谱-负化学离子化质谱法测定土壤中有机磷农药

用加速溶剂萃取法(ASE)萃取土壤中的有机磷农药,用气相色谱-负化学离子化质谱法(GC-NCI-MS)进行测定,并与气相色谱-电子轰击电离质谱法(GC-EI-MS)进行了对比。结果表明,EI法和NCI法均能满足目前的有机磷农药的分析需要。GC-EI-MS的适用范围比较广,操作比较简单;GC-NCI-MS在选择性和灵敏度等方面均具有较强优势。     

SPE-GC-MS法测定地下水中26种有机氯农药

采用固相萃取(SPE)技术,结合气相色谱/质谱(GC-MS)选择离子检测法(SIM)对水样中26种有机氯农药(OCPs)进行提取、净化、浓缩前处理,优选了固相萃取小柱填料及萃取、净化条件,优化了GC-MS的工作参数,建立了地下水中26种有机氯农药的SPE-GC-MS分析方法。针对不同的组分,本法加标回收率为76.422%~112.512%,相对标准偏差为4.905%~15.524%,检出限为0.014~0.089μg/L。该方法操作简单,消耗费用低,分析速度快,具有较高的灵敏度和回收率。     

Organic contamination of Italian and Tunisian culinary herbs and spices

Contaminants belonging to various classes, as polychlorobiphenyls, polycyclic aromatic hydrocarbons, organochlorine pesticides, organophosphorous pesticides, pyrethroid insecticides, fungicides, herbicides, synergists, carbamates, acaricides and insect growth regulators were simultaneously analysed by GC-MS/MS in 118 Italian and Tunisian culinary herbs and spices. The results obtained in Italian samples shown that laurel samples were the most contaminated with the presence of 15 residues on 140, whereas in rosemary (max value of 35?ng/g for cis-chlorfenyvinphos) and oregano (max value of 118.16?ng/g for ethion) some occasional residues can be observed, but always lower than the maximum residue levels; all the others samples shown no contamination. Among Tunisian samples, only rosemary contains a notably high content of pollutants exceeded the EU maximum residue limits (i.e., alachlor and phosalone with level of 359.2 and 43.3?ng/g, respectively), while oregano was determined to be free of contaminant residues. Considering the comparison among the different organic pollutants in Italian and Tunisian spices and herbs evaluated and the differences observed in this study a harmonization of regulation on contaminant residues in herbs and spices for human consumption should be needed, considering their increased use in diet and cooking.     

芦苇湿地对造纸废水中有机污染物的去除效果及机理

为了对芦苇湿地对造纸废水中有机污染物的去除效果及降解机理进行研究,本文采用GC-MS联用仪对经芦苇湿地处理前后造纸废水中有机污染物的组成和含量进行测定,并通过叠放色谱图的方法对造纸废水中有机污染物的降解效果进行分析。结果表明:(1)经芦苇湿地处理前造纸废水中共测出30种有机污染物,其中8种被列入美国EPA环境优先控制污染物黑名单。(2)纸浆造纸废水生物塘-芦苇湿地复合处理系统对有毒有机污染物基本上达到了较好的去除效果:有机污染物总量减少80%以上,且降解后的产物多为毒性较小的烷烃类。(3)利用质谱手段对有机污染物的降解规律进行了初步研究。该研究为造纸废水处理和资源化利用提供了科学依据,为"造纸废水-芦苇-造纸"生态纸业循环经济模式的进一步推广应用奠定了基础。     

VOCs走航监测:技术方法与案例应用

挥发性有机物(VOCs)来源广泛、组成复杂,是臭氧(O3)和二次有机气溶胶(SOA)的重要前体物,且其中一些组分对人体健康存在潜在威胁。VOCs的主要排放方式包括点源、面源和无组织源排放,排放过程具有瞬时性,难以控制和监测。与传统的离线监测和在线监测相比,走航监测技术具有监测范围大、响应快速、机动性强的特点,但中国VOCs的走航监测研究还鲜有报道。该研究通过使用装载了单质谱分析仪与便携式气相色谱-质谱联用仪(GC-MS)的走航车对珠三角沿海城市某工业集聚区进行VOCs走航监测,走航过程中对环境空气中的TVOCs进行快速监测并对TVOCs质量浓度高值点进行采样及VOCs组分的成分和浓度分析。该次走航共监测到32种优控污染因子和CW加油(加气)站、JH加油站、G空调电器生产企业的两器车间及南门货场等多个TVOCs质量浓度高值点,并通过分析进一步判断VOCs排放源。结合监测结果和实地调研推断:加油站的VOCs高值主要来源于油气挥发及机动车尾气排放;G空调企业的VOCs高值则主要来源于两器车间的喷涂、烘干、洗网工序及厂区内的机动车尾气排放。尽管VOCs走航监测技术目前还存在一定不足,该方法的应用能够为掌握区域VOCs污染现状及分布特征提供新的技术手段,为实现VOCs精细化管控提供新的思路。     

Volatile attractants for three Pteromalid parasitoids attacking concealed spruce bark beetles

Summary. The odour perceptive abilities, and preferences, of three bark beetle parasitoid species; Rhopalicus tutela (Walker), Roptrocerus mirus (Walker), and Roptrocerus xylophagorum (Ratzeburg) (Hymenoptera: Pteromalidae), were investigated to isolate and identify the essential compounds involved in host location. These parasitoids attack several economically important bark beetle species and oviposit preferentially on late larval stages concealed under the bark of conifers. Odours were collected from Norway spruce logs (Picea abies L. Karst.) containing Ips typographus L. (Coleoptera: Scolytidae) larvae. Biologically active compounds were isolated by coupled gas chromatographic-electroantennographic detection (GC-EAD), and identified by GC-mass spectrometry (GC-MS). Based on these analyses, four different synthetic baits were prepared and tested in a Y-tube walking bioassay. In the complex odour samples from spruce logs, only 16 compounds were EAD-active. The tested R. tutela and R. mirus females displayed similar trends in antennal activity to EAD-active compounds, responding mainly to oxygenated monoterpenes that indicate damaged conifers. Consequently, the synthetic baits were exclusively prepared with oxygenated monoterpenes. Parasitoid females (R. tutela and R. mirus) preferred spruce logs containing susceptible hosts over fresh logs, while male parasitoids (R. mirus) did not show any preference. However, when odours from fresh logs were mixed with synthetic baits (mimicking the odour composition of logs containing susceptible hosts), these combinations attracted female parasitoids (R. tutela, R. mirus, and R. xylophagorum). All synthetic baits seemed to be equally attractive to female parasitoids. Received 12 October 2000; accepted 18 January 2001     

维生素A合成废水难降解成分的定性分析及处理建议

采用吹扫捕集气相色谱-质谱法定性分析了维生素A生产企业污水处理厂的出水和现场中试出水中主要残留难降解成分。结果表明两种出水中10.7 min出峰的物质是含量最高最主要的难降解成分,是COD降不下去的最主要原因。结合维生素A合成工艺、这个物质的物理、化学性质、水样的颜色、气味确定了该物质是3-甲基-1-戊烯-4-炔-3-醇,并从可能的代谢途径分析了该物质难以降解的原因。并从合成工艺和污水处理工艺方面提出了污水处理的建议。     

我国大气VOCs监测现状及挑战

对我国开展大气VOCs监测的必要性、监测现状以及主要使用的监测方法进行了分析。目前,我国已初步建立了大气VOCs手工与自动监测网络,主要采用预浓缩-热脱附-气相色谱-质谱/氢火焰离子化检测器法进行PAMS组分和TO-15组分分析,利用高效液相色谱法进行13种醛、酮类组分分析。目前大气VOCs监测还存在数据质量、灵敏度有待提高,不同设备或方法监测结果一致性较差等问题。为此在VOCs监测过程中应进一步加强质量保证与质量控制,并尝试通过提高预浓缩装置除水和干扰物效率、提升进样量等多种手段提高监测灵敏度。     

气相色谱-质谱联用法在线观测大气中的氢氟碳化物和全氟化碳

利用组装的气相色谱-质谱联用系统(GC-MS)同时测定大气中6种氢氟碳化物(HFCs)和4种全氟化碳(PFCs),空气样品采样的时间分辨率120 min,精度范围0.15%—3.11%,准确度范围-1.52%—0.63%.对2011年2月在北京上甸子站的实验观测结果进行分析,获得HFC-23、HFC-32、HFC-134a、HFC-143a、HFC-125、HFC-152a、CF4、PFC-116、PFC-218、PFC-318的本底和非本底浓度,表明该系统适用于大气中HFCs和PFCs浓度在线观测.     

堆肥对土壤中石油烃的去除及微生物群落的影响

为研究堆肥对石油污染土壤中不同组分烃的去除作用及土壤微生物群落结构变化的影响,利用重量法和GC-MS测定土壤中总石油烃、烷烃和多环芳烃的含量,采用高通量测序技术研究了堆肥对土壤微生物群落结构和多样性的影响作用.结果表明,向石油污染土壤中施加堆肥进行42d的修复处理,土壤中石油烃、烷烃、多环芳烃去除率分别为（12.4±0.01）%、（10.2±0.01）%、（9.38±0.02）%;自然放置的土壤中3种烃去除率分别为（3.21±0.02）%、（-3.00±0.01）%、（-6.59±0.02）%.自然放置的土壤香农指数、ACE指数和Chao1指数分别为4.30、3489.3和2691.0,加入堆肥进行修复处理后,土壤香农指数、ACE指数和Chao1指数分别增加为5.80、4684.7和3851.8.油污土壤中放线菌门（Actinobacteria）所占丰度由47.3%降低为28.2%,拟杆菌门（Bacteroidetes）丰度由0.78%增加至16.2%.变形菌门（Proteobacteria）丰度为37.4%,修复结束后几乎不变.属水平上,油污土壤中的优势菌属包括原小单孢菌属（promicromonospora）、微小杆菌属（Exiguobacterium）、诺卡氏菌属（Nocardioides）、分支杆菌属（Mycobacterium）、柠檬酸细菌属（Citrobacter）.施入堆肥使土壤中的这些优势菌属丰度降低,土壤中出现氮单胞菌属（Azomonas）、藤黄单胞菌属（Luteimonas）、假鞘氨醇杆菌属（Pseudosphingo bacterium）、紫单胞菌属（Parapedobacter）等新菌属.研究结果表明,与自然放置的土壤相比,向石油污染土壤中施入有机堆肥可有效去除土壤中的石油烃、烷烃和多环芳烃.并使土壤微生物群落结构发生明显变化.