Release of sex pheromone and its precursors in the pine sawfly Diprion pini (Hym., Diprionidae)

Summary. The first identification of a sex pheromone of a pine sawfly (Hymenoptera, Diprionidae) dates back almost thirty years. Since then, female-produced pheromones of over twenty diprionid species have been investigated by solvent extraction followed by separation and identification. However, no study has shown what the females actually release. Collection of airborne compounds using absorbtion on charcoal filter as well as solid phase microextraction (SPME) followed by analysis employing gas chromatography combined with mass spectrometry (GC-MS), revealed an unusual system in Diprion pini, in which the pheromone precursor alcohol, 3,7-dimethyl-2-tridecanol, is released together with acetic, propionic, butyric and isobutyric acids. The corresponding acetate, propionate and butyrate esters of 3,7-dimethyl-2-tridecanol were also found in the samples. All esters were electrophysiologically active, and the propionate and isobutyrate were attractive in trapping experiments. Based on these and earlier reported results, it seems that at least in part of its range, the pheromone response of D. pini is not very specific with regard to the functional group, as long as this is an ester.     

SPE-GC-MS法对渤海水体中有机锡化合物的痕量分析

摘要：文中采用GC-MS仪器测定方法对海水中六种不同形态有机锡化舍物进行分析。在确定的GC-MS测定方法基础上得到SPE条件优化：选择NH。DDC鳌合剂,用5％的甲醇为携带剂,流速15ml／min,萃取温度45℃,萃取压力300bar,萃取时间为15min．     

固相微萃取-便携式GC/MS快速测定水中痕量有机磷农药

采用固相微萃取-便携式气相色谱/质谱联用法（In situ SPME/GC-MS）分析地表水和废水中6种有机磷农药，通过优化测定条件，使6种有机磷农药在200 μg/L~500 μg/L范围内线性良好。方法检出限为033 μg/L～122 μg/L，低、高质量浓度标准溶液6次测定结果的RSD为68%~175%，加标回收率为849%~109%，与实验室方法的测定结果基本一致。     

Utilization of long duration high-volume sampling coupled to SPME-GC-MS/MS for the assessment of airborne pesticides variability in an urban area (Strasbourg,France) during agricultural application

Atmospheric samples have been collected between 14 March and 12 September 2012 on a 2-week basis (15 days of sampling and exchange of traps each 7 days) in Strasbourg (east of France) for the analysis of 43 pesticides. Samples (particle and gas phases) were separately extracted using Accelerated Solvent Extraction (ASE) and pre-concentrated by Solid Phase Micro-Extraction (SPME) before analysis by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Four SPME consecutive injections at distinct temperatures were made in order to increase the sensitivity of detection for the all monitored pesticides. Currently used detected pesticides can be grouped in four classes; those used in maize crops (acetochlor, benoxacor, dicamba, s-metolachlor, pendimethalin, and bromoxynil), in cereal crops (benoxacor, chlorothalonil, fenpropimorph, and propiconazole), in vineyards (tebuconazole), and as herbicides for orchards, meadows of green spaces (2,4-MCPA, trichlopyr). This is in accordance with the diversity of crops found in the Alsace region and trends observed are in accordance with the period of application of these pesticides. Variations observed permit also to demonstrate that the long time sampling duration used in this study is efficient to visualize temporal variations of airborne pesticides concentrations. Then, long time high-volume sampling could be a simple method permitting atmospheric survey of atmospheric contamination without any long analysis time and consequently low cost.     

介孔涂层SPME- HPLC联用测定水样中的多环芳烃

以辛基键合SBA- 15为固相微萃取(SPME)的吸附涂层,考察了吸附和解吸时间、萃取温度、搅拌速率对SPME效率的影响,该方法的线性范围分别为0.4-300μg/L、4.0-450μg/L,检出限为0.3μg/L、0.10μg/L,以此方法测定了环境水样中萘、蒽的含量.该方法具有灵敏度高和精密度好的特点.     

Volatile organic compounds at swine facilities: A critical review

Volatile organic compounds (VOCs) are regulated aerial pollutants that have environmental and health concerns. Swine operations produce and emit a complex mixture of VOCs with a wide range of molecular weights and a variety of physicochemical properties. Significant progress has been made in this area since the first experiment on VOCs at a swine facility in the early 1960s. A total of 47 research institutions in 15 North American, European, and Asian countries contributed to an increasing number of scientific publications. Nearly half of the research papers were published by U.S. institutions.Investigated major VOC sources included air inside swine barns, in headspaces of manure storages and composts, in open atmosphere above swine wastewater, and surrounding swine farms. They also included liquid swine manure and wastewater, and dusts inside and outside swine barns. Most of the sample analyses have been focusing on identification of VOC compounds and their relationship with odors. More than 500 VOCs have been identified. About 60% and 10% of the studies contributed to the quantification of VOC concentrations and emissions, respectively. The largest numbers of VOC compounds with reported concentrations in a single experimental study were 82 in air, 36 in manure, and 34 in dust samples.The relatively abundant VOC compounds that were quantified in at least two independent studies included acetic acid, butanoic acid (butyric acid), dimethyl disulfide, dimethyl sulfide, iso-valeric, p-cresol, propionic acid, skatole, trimethyl amine, and valeric acid in air. They included acetic acid, p-cresol, iso-butyric acid, butyric acid, indole, phenol, propionic acid, iso-valeric acid, and skatole in manure. In dust samples, they were acetic acid, propionic acid, butyric acid, valeric acid, p-cresol, hexanal, and decanal. Swine facility VOCs were preferentially bound to smaller-size dusts.Identification and quantification of VOCs were restricted by using instruments based on gas Chromatography (GC) and liquid chromatography (LC) with different detectors most of which require time-consuming procedures to obtain results. Various methodologies and technologies in sampling, sample preparation, and sample analysis have been used. Only four publications reported using GC based analyzers and PTR-MS (proton-transfer-reaction mass spectrometry) that allowed continuous VOC measurement. Because of this, the majority of experimental studies were only performed on limited numbers of air, manure, or dust samples. Many aerial VOCs had concentrations that were too low to be identified by the GC peaks.Although VOCs emitted from swine facilities have environmental concerns, only a few studies investigated VOC emission rates, which ranged from 3.0 to 176.5 mg d⁻¹ kg⁻¹ pig at swine finishing barns and from 2.3 to 45.2 g d⁻¹ m⁻² at manure storages. Similar to the other pollutants, spatial and temporal variations of aerial VOC concentrations and emissions existed and were significantly affected by manure management systems, barn structural designs, and ventilation rates.Scientific research in this area has been mainly driven by odor nuisance, instead of environment or health concerns. Compared with other aerial pollutants in animal agriculture, the current scientific knowledge about VOCs at swine facilities is still very limited and far from sufficient to develop reliable emission factors.     

固相微萃取-车载气相色谱测定污染事故现场有机磷农药分析方法的探讨

探讨了在污染事故现场采用固相微萃取-车载气相色谱联用测定有机磷农药的分析方法，寻找出较适宜灵敏度与较短分析时间的最佳结合点，以适应污染事故应急现场测定有机磷农药的需求。该法完成一个样品的全部分析时问为30min，简便、高效，适用于应急现场5种有机磷农药的测定。     

固相微萃取-气相色谱-质谱法测定水中痕量有机磷和阿特拉津农药

采用PA萃取纤维吸附水中敌敌畏、乐果、内吸磷、甲基对硫磷、对硫磷、马拉硫磷等6种有机磷和阿特拉津农药,在气相色谱-质谱仪进样口热解吸后进行检测.筛选比较了几种萃取纤维,优化了萃取方式、萃取时间、离子强度、pH、解吸温度和解吸时间等萃取条件.方法适用于多类型水体中6种有机磷和阿特拉津农药的分析.     

固相微萃取-毛细管气相色谱法快速同步分析水中挥发性卤代烃及氯苯类化合物

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.本工作用固相微萃取富集水中挥发性卤代烃、氯苯类化合物,毛细管气相色谱分离分析,整个分析过程只需20min,检出限可达0.01～0.3μg/L,已用于自来水、地面水源中挥发性卤代烃、氯苯类化合物含量的测定.     

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。