GC法同时测定五香丸中丁香酚、去氢木香内酯及木香烃内酯含量

目的：建立GC法同时测定五香丸中丁香酚、去氢木香内酯及木香烃内酯含量的方法。方法：气相色谱条件：HP-5毛细管柱(30 m×0.25 mm×0.25μm);检测器：FID;进样口温度：230℃;检测器温度：250℃;程序升温,初始温度80℃,25℃/min升温至180℃,保持3 min,20℃/min升温至200℃,保持8 min;流速：1.0 mL/min,氢气流量40 mL/min,空气流量400 mL/min;分流进样,进样量1μL,分流比10∶1。结果：丁香酚、去氢木香内酯及木香烃内酯线性范围分别为16.99～45.31μg/mL、7.43～19.81μg/mL、12.76～34.02μg/mL,平均回收率分别为102.07%(RSD=0.75%)、97.85%(RSD=0.61%)、97.67%(RSD=0.76%)。结论：本研究所建立的方法可靠易行,专属性强,可以有效对五香丸中丁香及木香进行定量控制。     

GC法测定托吡司特中的水合肼残留量

建立一种气相色谱分析方法,测定托吡司特中的水合肼含量。采用DB-624毛细管色谱柱(30m×0.32mm,5μm);进样口温度为200℃;FID检测器,温度为250℃;升温程序:起始温度为95℃,保持5 min,再以10℃/min的速率升温至180℃,保持0 min,再以30℃/min的速率升温至225℃,保持4 min;载气为高纯氮气;进样量为1μL。结果显示二丙酮腙线性范围为0.00257～0.05135 mg·mL~(-1)(r=1.000);二丙酮腙平均回收率为101.4%,RSD为0.8%。该方法操作简便、快速准确,重复性好。     

气相色谱法测定红色正金软膏中薄荷脑的含量

目的建立红色正金软膏中薄荷脑含量测定的方法。方法采用气相色谱法测定红色正金软膏中薄荷脑的含量,色谱条件:HP-INNOWAX(0.25 mm×30 m,0.25μm)色谱柱;进样口温度250.0℃;初始柱温110.0℃,恒温5.0 min,以20.0℃/min升温至220.0℃,恒温4.0 min;载气为高纯氮气;FID检测器(280.0℃);分流比为10.0。结果薄荷脑在浓度0.005~0.030 g/m L范围内有良好的线性关系(R2=0.9999),重复性试验的RSD为0.309%,精密度试验的RSD为0.608%,稳定性试验的RSD为1.430%,加样回收率为99.16%~101.47%,RSD=0.897%。结论气相色谱法测定红色正金软膏中薄荷脑含量快速、简便、准确。     

苯胺及其衍生物的气相色谱分析方法研究

建立了气相色谱法对苯胺及其五种衍生物进行分离与同时测定的方法。最佳色谱分离条件如下:HP-5MS空心毛细管柱(30 m×0.32 mm×0.25μm);程序升温方式:初始温度70℃,以20℃/min升至150℃,保持1 min;以氮气为载气,流速为5.0 m L/min;尾吹气(氮气)流速为30 m L/min;氢气流速为35 m L/min;空气流速为400 m L/min;不分流进样,进样量为1μL;进样口温度为260℃,检测器温度为320℃。在最佳实验条件下,六种组分在4 min内全部出峰,达到较好的分离,实现对组分的分离与同时检测。     

气相色谱法测定牛磺熊去氧胆酸原料药中的残留溶剂

目的建立测定牛磺熊去氧胆酸原料药中丙酮、乙酸乙酯、乙醇、四氢呋喃4种残留溶剂含量的检测方法。方法采用Agilent DB-624毛细管柱(30 m×0.53 mm,3μm);氢离子火焰检测器(FID);进样口温度为230℃;检测器温度为250℃;柱温采用程序升温:起始温度为40℃,维持4 min;以10℃/min速率升温至90℃;以40℃/min的速率升温至200℃,维持3 min;载气为氮气,样品溶剂为N,N-二甲基甲酰胺(DMF),进样量1μL。结果 4种有机溶剂均达到完全分离,在考察的浓度范围内线性关系良好,精密度和回收率好。结论本方法简便、灵敏,准确性高,可用于牛磺熊去氧胆酸原料药残留溶剂的测定。     

气相色谱法测定聚桂醇400中月桂醇含量

建立气相色谱方法用于测定聚桂醇400原料药中月桂醇的残留量。采用BD-5ht(30 m×0.25 mm,0.1μm)毛细管色谱柱,程序升温,起始温度120℃,维持1 min,以10℃/min的速度升至350℃,维持10 min,进样口温度300℃,分流进样,分流比50∶1,FID检测器,检测器温度350℃,进样量1 u L。结果显示,月桂醇的回归方程为A=1.2743×103c+1.2867(r=0.9998),线性范围为0.2039~0.6118 mg·m L-1,月桂醇含量为1.65%。综上所述,该方法简单易行,结果稳定准确,适用于聚桂醇400原料药中月桂醇含量的测定。     

气相色谱法测定蕲艾移栽品中桉油精的含量

建立了一种利用气相色谱法快速测定艾叶中桉油精含量的方法。气相色谱柱为HP-5毛细管柱(30 m×0.32 mm,0.25μm);氢火焰离子化检测器(FID)温度为250℃;进样口温度:240℃;程序升温:柱温起始温度为50℃,以5℃/min升至75℃,保持6 min,再以20℃/min升至200℃,保持3 min。该方法操作简单、快捷,精密度、重复性、稳定性、准确度的RSD≤1.83%;平均加样回收率为96.03%,RSD为1.78%(n=6)。蕲艾在湖南的移栽品桉油精含量变化不大。     

气相色谱法测定速效救心丸中龙脑的含量

目的:建立速效救心丸中龙脑含量测定的方法。方法:采用气相色谱法测定速效救心丸中龙脑的含量,色谱柱:HP-INNOWAX(30m×0.25 mm×0.25μm)毛细管色谱柱;检测器:火焰离子化检测器(FID);柱温140℃,进样口温度190℃,检测器温度220℃;载气为N2,流速为1.0 mL/min;结果:龙脑的峰面积与其浓度在0.02133~0.2133 mg/mL范围内呈良好的线性关系,相关系数R2=0.9990(n=6);加样回收率为98.2%~99.8%(RSD=0.5%,n=9)。结论:本文采用的气相色谱法操作简便、准确、重现性好,可用于该药的龙脑含量测定。     

气相色谱法测定舒必利原料药中甲醇、乙醇的残留量

目的:建立气相色谱法测定舒必利原料药中甲醇、乙醇残留量。方法:以DB-624(30 m×0.53 mm×3.0μm)为色谱柱,程序升温;氮气为载气;流速为每分钟4.0 m L;检测器为FID检测器,检测器温度为250℃;进样口温度为140℃;进样量为1μL;分流比为5∶1。结果:甲醇在2.068～310.2μg/m L范围内线性关系良好(r=0.999),乙醇在4.132～619.8μg/m L范围内线性关系良好(r=0.999);甲醇回收率为99.7%,RSD为0.63%;乙醇回收率为100.8%,RSD为0.83%。结论:本方法测定舒必利原料药中甲醇、乙醇的残留量,方法灵敏、准确,优于现有检测方法,有利于提高药品的安全性。     

气相色谱法测定环己酮中的微量轻组分

采用气相色谱法测定环己酮中微量轻组分含量,探讨了色谱柱、柱温、气化温度、检测温度、载气流量对环己酮及其组分色谱分离的影响。结果表明:选用强极性毛细管色谱柱AB-Wax 60 m×0.32 mm×0.5μm,采用程序升温法,以升温速率20℃/min升温至色谱柱初始温度100℃,保持时间10 min,再以10℃/min升至色谱柱终温150℃,保持时间30 min,在进样口温度为250℃,氢火焰离子化检测器温度为280℃,载气为氮气,流量为1.5 mL/min,进样量为0.6μL的条件下,采用气相色谱仪测定环己酮中微量轻组分含量,环己酮中微量轻组分能得到很好地分离,通过峰面积外标法定量,测定结果的加标回收率为96.3%～97.2%,相对标准偏差为0.86%～1.13%。     

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.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

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.     

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.     

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。