固相萃取-气相色谱/质谱法同时测定海水中9种硝基苯类化合物

建立了固相萃取-气相色谱/质谱(GC/MS)同时测定海水中9种硝基苯类化合物的分析方法。海水样品经Oa-sisHLB固相萃取小柱萃取富集,正己烷/丙酮洗脱,采用GC/MS进行定性定量,线性响应良好,基体干扰小,方法检出限在0.03～0.10μg/L(按采样1 L水计),添加回收率在72.8%～116%,精密度为1.2%～5.4%,并利用该方法对广西近岸海域6个点位实际海水样品进行了监测。该方法可以同时满足海水中9种硝基苯类化合物的测定。     

Determination of Acaricide Residues in Saudi Arabian Honey and Beeswax Using Solid Phase Extraction and Gas Chromatography

Determination of acaricide residues of flumethrin, tau-fluvalinate, coumaphos, and amitraz in honey and beeswax was carried out using a rapid extraction method utilizing C-18 SPE cartridges and an analytical method utilizing GC with ECD, NPD, and MSD detectors for the four acaricides. Recovery percentages from the extraction method ranged from 90–102%, while the minimum detection levels ranged from 0.01–0.05 mg/kg for the acaricides. Nine of the 21 analyzed samples were found to be contaminated with the acaricides tau-fluvalinate and coumaphos. Neither flumethrin nor amitraz was detected in any of the honey or wax samples. Coumaphos was found only in honey samples in which two samples exceeded the tolerance levels set by EPA and EC regulations. It has not been detected in beeswax. Five honey samples and eight beeswax samples were found to be contaminated with tau-fluvalinate. One of the wax samples was contaminated with a relatively high residue of tau-fluvalinate and contained above 10 mg/kg.     

冀西北典型北方小城镇污水处理厂中抗生素的分布和去除

抗生素在环境中作为一种新型污染物,是目前污水处理厂中重要的污染物之一.为考察小城镇污水处理厂对抗生素的去除效果,选择3种典型小城镇污水处理工艺(CASS、A~2/O及Orbal氧化沟工艺),研究了4种四环素类、3种β-内酰胺类、4种大环内酯类、3种喹诺酮类和2种磺胺类在进出水中的浓度分布、去除情况以及不同工艺抗生素去除效率,并对抗生素浓度与水质常规指标的相关性进行分析.结果表明,所研究的污水处理厂中氧氟沙星和诺氟沙星为主要抗生素,并且去除效果较好.5个污水处理厂运行情况良好,CASS工艺和Orbal氧化沟工艺对大部分抗生素的去除效果比A~2/O工艺好,抗生素去除率均能达到60%以上.同时,发现CASS工艺和A~2/O工艺对β-内酰胺类(氨苄西林、青霉素)、喹诺酮类(恩诺沙星、氧氟沙星和诺氟沙星)和大环内酯类(克拉霉素)的去除效果最好,Orbal氧化沟工艺对四环素类(四环素、土霉素)和磺胺类(磺胺嘧啶)的去除效果最好.将抗生素浓度和水质基本参数(NH_4~+-N、TN、COD、pH等)进行相关性分析后,发现抗生素浓度与水质基本参数NH_4~+-N、COD呈一定正相关,污染物浓度越高,红霉素(EM)、罗红霉素(ROX)、差向四环素盐酸盐(ETC)、克拉霉素(CLR)、环丙沙星(CIP)、氧氟沙星(OFX)、差向土霉素(E-OTC)、四环素(TC)、土霉素(OTC)以及诺氟沙星(NOR)的浓度也相对更高,这为确保小城镇污水厂的稳定运行,降低抗生素类污染物的生态风险提供了重要参考.     

环境样品阿特拉津及降解产物分析方法进展

阿特拉津是一种世界范围广泛使用的除草剂。文章介绍了环境样品中阿特拉津及其降解产物分析的前处理技术和分析方法的研究进展,并为今后的研究方向提出了建议。     

固相微萃取-毛细管气相色谱法快速同步分析水中硝基苯类及氯苯类化合物

固相微萃取是一种快速、简便、集萃取浓缩进样于一体的样品前处理技术,具有分析时间短、灵敏度高、无需有机溶剂的优点。文章用固相微萃取富集水中9种硝基苯类及5种氯苯类化合物,毛细管气相色谱ECD检测器分离分析,整个分析过程只需25min,检出限可达0.0002~0.02μg/L,已用于地表水、海水与工厂废水中硝基苯类及氯苯类化合物含量的测定。     

便携式气相色谱法测定室内空气中的苯系物

介绍了FFKM301便携式气相色谱仪在室内空气苯系物现场监测中的应用,通过对便携式气相色谱仪柱温、压力、泵抽时间和反吹时间等条件的讨论,确定了最佳的方法设置:柱温60℃、压力12psi、泵抽时间20s、反吹时间300s,该方法的检出限为10ppb(苯),精密度小于6%,与经典的气相色谱法进行对比试验,相对偏差不超过20%,能够满足室内空气苯系物的监测要求。     

GC-MS测定土壤中酞酸酯类化合物

采用毛细管柱气相色谱-质谱联用选择离子检测(GC-MS-SIM)技术,结合快速萃取和佛罗里硅土柱净化方法分析土壤中的六种酞酸酯类(PAEs)化合物。结果表明,六种PAEs峰形好,平均加标回收率为76.7%~110%,相对标准偏差为2.5%~4.5%。方法具有操作简便、回收率高、纯化效果好和对环境友好的特点,且具有很强的实用性。     

Tissue distribution of polychlorinated naphthalenes (PCNs) and non-ortho chlorinated biphenyls (non-ortho CBs) in harbour porpoises (Phocoena phocoena) from Swedish waters

Polychlorinated naphthalenes (PCNs) and non-ortho chlorinated biphenyls (non-ortho CBs) were analysed in blubber, nuchal fat, liver, muscle, kidney and brain of three male harbour porpoises (Phocoena phocoena) from the west coast of Sweden. To estimate spatial variation, PCNs and non-ortho CBs were analysed in six blubber samples collected at different anatomical sites of each animal. Highest wet weight concentrations of ΣPCNs were detected in the lipid rich tissues (blubber and nuchal fat) and liver (520–730 and 520 pg/g, respectively) and lowest in brain (22 pg/g). TetraCNs were most abundant in muscle, kidney and brain, while the hexaCNs were most abundant in the lipid rich tissues and liver. The highest lipid weight concentration recorded (11 ng/g) was for the hexaCN congeners no. 66/67 in liver. These coeluting hexaCN congeners accounted for 80–100% of total hexaCNs in all tissues examined.

Concentrations of Σnon-ortho CBs were highest in lipid rich tissues (220–280 pg/g wet weight). Non-ortho CB no. 77 and 169 constituted between 62–86% and 4.9–9.3%, respectively, of total Σnon-ortho CBs. No major variation of Σnon-ortho CB concentrations was found between the six different blubber sites but higher ΣPCN concentrations (wet weight) were found dorsally at the peduncle. Toxic equivalent concentrations (TEQs) showed that non-ortho CB no. 126 was the main contributor to total TEQs in all tissues, except liver in which hexaCN congener nos. 66/67 contributed to about 50% of total TEQs.     

水解酸化-缺氧法处理采油废水的污染物迁移降解试验研究

水解酸化-缺氧法对采油废水有较好的处理效果,采用GC/MS技术对水解酸化-缺氧法处理采油废水过程中污染物的迁移降解进行的研究表明:水解酸化段和缺氧段对采油废水中碳原子为C6～C9、分子量为100～140的有机物均有较好的降解能力.其中,在水解酸化段中酮类、芳烃得到较好的降解,缺氧段中酚类和醚类化合物降解明显.水解酸化-缺氧工艺对于采油废水中的甲苯和二甲苯具有较好的降解能力.     

城市垃圾焚烧炉飞灰中多环芳烃分析研究

报道了气相色谱/质谱分析垃圾焚烧厂飞灰样品中多环芳烃的分析方法和分析结果,建立了气相色谱/质谱分析垃圾焚烧厂飞灰样品中多环芳烃的分析方法。方法的加标回收率基本在80%～110%之间。