SPE-UPLC-Q-TOF/MS测定水环境中的雌激素

研究建立了固相萃取、超高效液相色谱-四极杆串联飞行时间质谱(UPLC-Q-TOF/MS)测定水环境中6种雌激素(雌三醇、雌二醇、炔雌醇、雌酮、己烯雌酚、双酚A)的分析方法。水样经甲醇活化后的C18固相萃取小柱富集浓缩,用10 mL 10%的甲醇溶液淋洗,10 mL纯甲醇洗脱,洗脱液经高纯氮气吹至0.4 mL后用UPLC-Q-TOF/MS测定。6种常见的雌激素质量浓度在0.5~100μg/L范围内时,具有良好的线性(R0.993 7),检出限介于5.60~10.6 ng/L之间。空白加标水样为1μg/L的水平下,相对标准偏差(RSD)为2.8%~9.0%,其加标回收率为75%~101%。该方法可用于水体中雌激素的分析测定。     

凝固分散液液微萃取-HPLC法测定水中萘芴菲

建立了凝固分散液液微萃取(SFO-DLLME)-高效液相色谱法(HPLC)测定水中萘、芴和菲的新方法。以1-十二醇为萃取剂,甲醇为分散剂,优化了影响SFO-DLLME萃取效率的因素。在最佳条件下,萘、芴和菲的检出限分别为0.011、0.056、0.049μg/L,萘的线性范围为0.1~50.0μg/L,芴和菲的线性范围为1.0~500μg/L。实际水样加标回收率78.6%~95.1%,相对标准偏差(n=5)3.9%~7.2%。方法简便快速,灵敏度高,环境友好,成功用于实际水样分析。     

分散液液微萃取-分光光度法测定水中痕量铜

以氯仿为萃取剂,乙腈为分散剂,新铜试剂为螯合剂,建立了水中痕量铜分散液液微萃取分光光度法测定的新方法。研究了萃取剂、分散剂、络合剂的用量、p H、萃取时间等影响因素。在最佳条件下,方法的线性范围为1.0~200μg/L,相关系数(r)为0.998 4,检出限为0.35μg/L,对100μg/L的铜离子进行11次平行测定的相对标准偏差为3.42%,加标回收率为96.2%~101.7%。方法可应用于水样中痕量铜含量的测定。     

全自动固相萃取-气相色谱/质谱法测定水中的甲萘威

[目的]建立了全自动固相萃取-气相色谱/质谱联用测定水体中甲萘威的方法。[方法]优化了固相萃取的条件,采用ProElut PLS固相萃取柱,以甲醇作为洗脱溶剂萃取水样中的甲萘威,用气相色谱/质谱法测定。[结果]甲萘威质量浓度在5.0~250.0μg/L范围内与其气相色谱/质谱响应值线性关系良好,相关系数为0.9999,检出限为0.022μg/L。样品加标回收率在90.2%~92.5%之间,测定结果的相对标准偏差为1.9%~3.2%。[结论]该方法自动化程度高、快速、准确,适合于水中甲萘威的测定。     

磁性固相萃取-高效液相色谱串联三重四级杆质谱法测定环境水样中的磺胺类抗生素残留

建立了磁性固相萃取-高效液相色谱串联三重四级杆质谱法分析环境水样中的磺胺类抗生素残留的方法。优化后的磁性固相萃取条件:将50 mg磁性萃取材料加入100 m L水样,调节水样pH至4,振荡萃取20 min后利用外加磁场收集磁性萃取材料,再用4 m L甲醇(含1%氨水)涡旋洗脱,分离洗脱液氮吹至干,用液相色谱初始流动相定容后进行高效液相色谱-串联质谱分析。4种磺胺类抗生素在5~500μg/L范围内线性良好,相关系数均大于0.999,检出限为4.2~4.7μg/L,加标回收率为72.3%~88.5%,相对标准偏差在3.5%~10.2%之间。该方法简单便捷、用时短、重现性好、有机试剂消耗少,能够应用于实际水样中磺胺类抗生素的检测。     

浊点萃取分光光度法测定水样中痕量铁

建立了浊点萃取-分光光度法测定痕量铁的新方法。详细考察了溶液的pH值、螯合剂和表面活性剂浓度、平衡温度和时间等条件对浊点萃取效果的影响。该方法的线性范围为6.0~500μg/L(r=0.9996),检出限为1.58μg/L,加标回收率为98.7%~101.6%,相对标准偏差为1.3%~2.2%。该方法已成功应用于实际水样分析。     

分散固相萃取-UHPLC-MS/MS法测定水中5种苯脲类除草剂

建立分散固相萃取-超高液相色谱串联质谱(UHPLC-MS/MS)同时测定环境水样中5种苯脲类除草剂(敌草隆、利谷隆、灭草隆、异丙隆、绿麦隆)残留的分析方法。考察了吸附剂的种类与数量、水样pH、吸附剂的种类和体积等条件对除草剂回收率的影响。在最佳实验条件下,5种苯脲类除草剂在0.01~5.0μg/L范围内呈良好的线性关系(0.999 3~0.9999),方法检出限为2.04~3.12 ng/L。对环境水样的加标回收率分别为78.2%~108.3%,相对标准偏差RSD分别为6.8%~11.2%。本方法操作简便快速、稳定性好、灵敏度高,能够满足环境水体中苯脲类除草剂残留的分析要求。     

分散液液微萃取-分光光度法测定水中痕量铜

以氯仿为萃取剂,乙腈为分散剂,新铜试剂为螯合剂,建立了水中痕量铜分散液液微萃取分光光度法测定的新方法。研究了萃取剂、分散剂、络合剂的用量、p H、萃取时间等影响因素。在最佳条件下,方法的线性范围为1.0²00μg/L,相关系数(r)为0.998 4,检出限为0.35μg/L,对100μg/L的铜离子进行11次平行测定的相对标准偏差为3.42%,加标回收率为96.2%200μg/L,相关系数(r)为0.998 4,检出限为0.35μg/L,对100μg/L的铜离子进行11次平行测定的相对标准偏差为3.42%,加标回收率为96.2%¹01.7%。方法可应用于水样中痕量铜含量的测定。     

悬浮固化分散液液微萃取光度法测定痕量锌

采用悬浮固化分散液液微萃取(DLLME-SFO)分光光度法测定水样中痕量锌。以1-(2-吡啶偶氮)-2-萘酚(PAN)为配位剂,密度小于水,凝固点为24℃的十二醇为萃取剂,乙醇为分散剂,对水样进行分散液液微萃取。对萃取剂和分散剂的类型和体积、溶液的p H、PAN的用量、萃取时间等参数进行了优化。方法的线性范围5.0~800μg/L,检出限0.62μg/L,富集倍数50倍,应用于测定水样中痕量锌,回收率为96%~98.7%。     

不锈钢丝SPME-HPLC联用测定水样中的芳香烃

在修饰过的不锈钢丝表面涂覆(苯乙烯-二乙烯基苯)高内相乳液,制作了不锈钢丝固相微萃取(SPME)萃取头,与高效液相色谱(HPLC)联用测定了环境水样中的芳香烃。系统考察了萃取时间及解吸时间等实验条件对萃取效率的影响,建立了测定环境水样中芳香烃的SPME-HPLC方法。实验结果表明,方法的柱内(n=6)和柱间(n=3)精密度(RSD)分别小于6.5%和8.6%,实际样品的加标回收率在84.4%~95.4%之间;3种芳香烃化合物的线性范围为5~200μg/L,线性相关系数r>0.9960,检出限在0.09~0.20μg/L之间。该方法快速、灵敏、简便,适用于快速分析环境水样中的芳香烃。     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Methyl 2,4,6-decatrienoates Attract Stink Bugs and Tachinid Parasitoids

Halyomorpha halys (Stål) (Pentatomidae), called the brown marmorated stink bug (BMSB), is a newly invasive species in the eastern USA that is rapidly spreading from the original point of establishment in Allentown, PA. In its native range, the BMSB is reportedly attracted to methyl (E,E,Z)-2,4,6-decatrienoate, the male-produced pheromone of another pentatomid common in eastern Asia, Plautia stali Scott. In North America, Thyanta spp. are the only pentatomids known to produce methyl 2,4,6-decatrienoate [the (E,Z,Z)-isomer] as part of their pheromones. Methyl 2,4,6-decatrienoates were field-tested in Maryland to monitor the spread of the BMSB and to explore the possibility that Thyanta spp. are an alternate host for parasitic tachinid flies that use stink bug pheromones as host-finding kairomones. Here we report the first captures of adult and nymph BMSBs in traps baited with methyl (E,E,Z)-2,4,6-decatrienoate in central Maryland and present data verifying that the tachinid, Euclytia flava (Townsend), exploits methyl (E,Z,Z)-2,4,6-decatrienoate as a kairomone. We also report the unexpected finding that various isomers of methyl 2,4,6-decatrienoate attract Acrosternum hilare (Say), although this bug apparently does not produce methyl decatrienoates. Other stink bugs and tachinids native to North America were also attracted to methyl 2,4,6-decatrienoates. These data indicate there are Heteroptera in North America in addition to Thyanta spp. that probably use methyl 2,4,6-decatrienoates as pheromones. The evidence that some pentatomids exploit the pheromones of other true bugs as kairomones to find food or to congregate as a passive defense against tachinid parasitism is discussed.     

2005～2006年国外塑料工业进展

收集了2005年7月～2006年6月国外塑料工业的相关资料，介绍了2005—2006年国外塑料工业的发展情况。提供了世界塑料产量、消费量及全球各类树脂生产量以及各国塑料制品的进出口情况。作为对比，介绍了中国塑料的生产情况。按通用热塑性树脂（聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂）、工程塑料（聚酰胺、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚）、通用热固性树脂（酚醛、聚氨酯、不饱和树脂、环氧树脂）、特种工程塑料（聚苯硫醚、液晶聚合物、聚醚醚酮）的品种顺序，对树脂的产量、消费量、供需状况及合成工艺、产品开发、树脂品种的延伸及应用的扩展作了详细的介绍。     

2007～2008年世界塑料工业进展

收集了2007年7月～2008年6月世界塑料工业的相关资料,介绍了2007～2008年国外塑料工业的发展情况,提供了世界塑料产量、消费量及全球各类树脂的需求量及产能情况.按通用热塑性树脂(聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂)、工程塑料(尼龙、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚)、特种工程塑料(聚苯·硫醚、液晶聚合物、聚醚醚酮)、通用热固性树脂(酚醛、聚氨酯、不饱和聚酯树脂、环氧树脂)不同品种的顺序,对树脂的产量、消费量、供需状况及合成工艺、产品应用开发、树脂品种的延伸及应用的进一步扩展等技术作了详细介绍.     

Inorganic/organic nanocomposite coatings: The next step in coating performance

Inorganic/organic hybrid materials have considerable promise and are beginning to become a major area of research for many coating usages, including abrasion and corrosion resistance. Our primary approach is to prepare the inorganic phase in situ within the film formation process of the organic phase. The inorganic phase is introduced via sol-gel chemistry into a thermosetting organic phase. By this method, the size, periodicity, spatial positioning, and density of the inorganic phase can be controlled. An important aspect of the inorganic/organic hybrid materials is the coupling agent. The initial task of the coupling agent is to provide uniform mixing of the oligomeric organic phase with the sol-gel precursors, which are otherwise immiscible. UV-curable inorganic/organic hybrid systems have the advantages of a rapid cure and the ability to be used on heat sensitive substrates such as molded plastics. Also, it is possible to have better control of the growth of the inorganic phase using UV curing. It is our ultimate goal to completely separate the curing of inorganic and organic phases to gain complete control over the morphology, and hence optimization of “all” the coating properties. Thus far, it has been found that concomitant UV curing of the inorganic and organic phases using titanium sol-gel precursors afforded nanocomposite coatings which completely block the substrate from UV light while maintaining a transparent to visible light. Also, it has been found that the morphology of the inorganic phase is highly dependent on the concentration and reactivity of the coupling agent. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004, in Chicago, IL.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Some Large Wood-Boring Beetles in Southeastern USA

Ethanol and α-pinene were tested as attractants for large wood-boring pine beetles in Alabama, Florida, Georgia, North Carolina, and South Carolina in 2002–2004. Multiple-funnel traps baited with (−)-α-pinene (released at about 2 g/d at 25–28°C) were attractive to the following Cerambycidae: Acanthocinus nodosus, A. obsoletus, Arhopalus rusticus nubilus, Asemum striatum, Monochamus titillator, Prionus pocularis, Xylotrechus integer, and X. sagittatus sagittatus. Buprestis lineata (Buprestidae), Alaus myops (Elateridae), and Hylobius pales and Pachylobius picivorus (Curculionidae) were also attracted to traps baited with (−)-α-pinene. In many locations, ethanol synergized attraction of the cerambycids Acanthocinus nodosus, A. obsoletus, Arhopalus r. nubilus, Monochamus titillator, and Xylotrechus s. sagittatus (but not Asemum striatum, Prionus pocularis, or Xylotrechus integer) to traps baited with (−)-α-pinene. Similarly, attraction of Alaus myops, Hylobius pales, and Pachylobius picivorus (but not Buprestis lineata) to traps baited with (−)-α-pinene was synergized by ethanol. These results provide support for the use of traps baited with ethanol and (−)-α-pinene to detect and monitor common large wood-boring beetles from the southeastern region of the USA at ports-of-entry in other countries, as well as forested areas in the USA.