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。     

气相色谱法测定不同配伍比例三棱、莪术药对莪术醇、莪术二酮的含量

目的:建立测定不同配伍比例三棱、莪术药对中莪术醇、莪术二酮含量的方法,探讨不同比例配伍的药对的合理性。方法:色谱柱Agilent HP-5柱(30 m×250μm,0.25μm);进样口温度220℃;检测器(FID)温度270℃,载气∶高纯氮气,流量30 m L·min-1,空气300 m L·min-1,氢气m L·min-1。程序升温条件:初始温度50℃,以5℃/min升温速率升至125℃,恒温1 min后,以1℃/min速率升至134℃,再以5℃/min升温速率升至250℃,恒温10 min,进样量为1μL。结果:莪术醇、莪术二酮分别在2.584~33.408μg(r=0.9991),1.216~14.592μg(r=0.9991)范围有良好的线性关系。莪术醇、莪术二酮加样回收率(n=6)分别为99.2%,98.9%,RSD均3%。三棱、莪术药对4个配伍比例(1∶1、1∶2、2∶1、0∶1)中三棱、莪术2∶1时莪术醇、莪术二酮溶出量最高。结论:该方法简便、准确,可测定三棱、莪术药对莪术醇、莪术二酮的含量,为其质量控制提供参考。     

RP-HPLC法测定奥利司他原料药的含量

建立奥利司他原料药的含量测定方法。采用高效液相色谱法,Agilent SB-C18色谱柱(25cm×4.6mm,5μm),流动相为甲醇∶水(90∶10);柱温为30℃;流速1.0m L·min-1;进样量20μL。紫外检测器,检测波长为190 nm。主成分奥利司他在0.4~0.6 mg/m L浓度范围内线性关系良好,相关系数r0.999,在相对浓度80%、100%、120%范围内的平均回收率较高。该检测方法精密度及准确度较高,可订入奥利司他原料药的质量标准中,作为含量测定的控制方法。     

气相色谱法测定尼可地尔原料药中乙二醇的残留量

目的:建立气相色谱法测定尼可地尔原料药中乙二醇残留量。方法:以DB-WAXETR(30 m×0.53 mm×1.0μm)为色谱柱,程序升温;氮气为载气;流速为每分钟5.0 mL;检测器为FID检测器,检测器温度为260℃;进样口温度为140℃;进样量为1μL;分流比为10∶1。结果:乙二醇在6.389～76.668μg/mL范围内线性关系良好(r=0.9991),回归方程为Y=0.593X-0.8867;回收率为98.28%,RSD为4.3%;检出限为0.62μg/mL,定量限为6.2μg/mL。结论:本方法测定尼可地尔原料药中乙二醇的残留量,方法灵敏、准确,有利于提高药品的安全性。     

普拉格雷含量及有关物质的测定

采用HPLC法测定了普拉格雷原料药含量和有关物质。色谱条件如下:色谱柱为C18柱(150mm×4.6mm,5μm),柱温30℃,流动相为乙腈-磷酸盐缓冲溶液(pH值5.0)(50∶50,体积比),流速1.0mL·min-1,检测波长219nm,进样量10μL。结果表明:普拉格雷在0.5~3.0μg·mL-1范围内,线性关系良好,平均加样回收率为99.95%(n=9)。此法操作简便、快速、灵敏、准确,样品处理简便易行,可用于测定普拉格雷原料药含量和有关物质。     

HPLC法测定青荚叶中的木犀草素和肉桂酸的含量

建立测定青荚叶中木犀草素、肉桂酸含量的HPLC测定方法。采用反相高效液相色谱法(RP-HPLC),色谱柱为Thermo C18柱(250 mm×4.6 mm,5μm),测定木犀草素:流动相为甲醇∶0.2%磷酸水溶液(55∶45),流速1.0 m L/min,进样量20μL,检测波长350 nm;测定肉桂酸:流动相为甲醇∶1.67%冰醋酸水溶液(50∶50),流速1.0 m L/min,进样量20μL,检测波长270 nm。结果表明,木犀草素进样量在3.4~54.4μg范围内,其峰面积与浓度呈良好的线性关系(R2=0.999 9),样品回收率为99.67%,肉桂酸进样量在0.24~2.4μg范围内,其峰面积与浓度呈良好的线性关系(R2=0.999 4),样品回收率为93.64%。方法专属性强,准确可靠,可用于青荚叶中木犀草素、肉桂酸的含量测定。     

HPLC测双氯芬酸钾干混悬剂的含量

建立了高效液相色谱法测定双氯芬酸钾干混悬剂含量的测定方法。色谱柱为Kromasil C18(250 mm×4.6 mm,2.5μm),流动相:甲醇-水-冰醋酸(80∶20∶0.8,V∶V∶V),检测波长为276 nm,流速为1.0 m L·min-1,进样量为20μL。结果表明:y=40999x+119667(r=0.9995,n=7)线性范围为4.0~6.0μg·m L-1;最低检测限为1.66 ng,定量限为5.56 ng;平均回收率为99.57%。该方法简便、准确、适用于双氯芬酸钾干混悬剂的含量测定。     

高效液相色谱法和电位滴定法测定盐酸萘甲唑啉原料药含量

目的:分别建立电位滴定法和高效液相色谱法测定盐酸萘甲唑啉原料药含量。方法:高效液相色谱法采用Waters XBridge C18色谱柱(4.6 mm×250 mm,5μm),流动相为磷酸二氢钾缓冲液(取3.0 g磷酸二氢钾,加水800 m L使溶解,加3.0 m L三乙胺,用磷酸调节pH值至3.0,加水稀释至1000 m L)-乙腈(80∶20,体积比),流速为1.0 m L·min-1,检测波长280 nm,柱温30℃。电位滴定法以乙醇为溶剂,用氢氧化钠标准溶液(0.1 mol·L-1)滴定,电位法判定终点。结果:高效液相色谱法:在0.02～76μg·m L-1范围内线性关系良好,r=0.9998;方法精密度RSD为0.3%(n=6);平均回收率为100.2%(n=9),RSD为0.5%。电位滴定法:在0.12～0.25 g范围内线性关系良好,r=0.9998;方法精密度RSD为0.15%(n=6);平均回收率为100.2%(n=9),RSD为0.15%。结论:电位滴定法和高效液相色谱法的含量测定结果无显著性差异,均可用于盐酸萘甲唑啉含量测定。HPLC法相较于电位滴定法,专属性高,精密度好,使用样品量少,有利于环保,故推荐首选HPLC法。     

HPLC法测定索非布韦原料药的含量

目的:采用HPLC法测定索非布韦的含量。方法:采用色谱柱C18(150 mm×4.6 mm×5μm)为色谱柱,以0.05%磷酸溶液为流动相A,乙腈∶甲醇=80∶20为流动相B,以流动相A∶流动相B(80∶20)等度洗脱,流速为1.0 m L/min。稀释液为p H=2.0磷酸水溶液∶乙腈=80∶20,检测波长为260 nm,柱温为35℃。结果:索非布韦的线性范围为80.928~121.392μg/m L;3批样品中索非布韦的含量分别为99.7%、99.8%、99.7%。结论:本方法简便、准确,适用于索非布韦含量的测定。     

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。