HPLC法测定铁甲草中大黄素的含量

建立铁甲草中大黄素的含量测定方法。采用高效液相色谱法(HPLC)测定铁甲草中大黄素的含量,应用Waters XBridgePeptide BEH C18(4. 6 mm×250 mm,5μm)色谱柱,以甲醇-0. 1%甲酸(85∶15)为流动相,流速1. 0 m L/min,柱温35℃,进样量为10μL,检测波长254 nm,测定大黄素的含量。大黄素浓度在5～50μg/m L范围内呈良好线性关系(Y=38315X-16555,R2=0. 9994),平均回收率为98. 94%,RSD为1. 98%(n=6)。本文方法准确灵敏、稳定可靠,可用于铁甲草中大黄素的含量测定。     

HP LC测定处方中大黄素和大黄酚的含量

建立测定处方中大黄素和大黄酚含量的高效液相色谱法。固定相为依立特C_(18)柱(5μm,4.6 mm×250 mm),流动相为甲醇-0.1%磷酸溶液(85∶15,V/V),流速为1 mL/min;柱温为30℃,检测波长为240 nm。大黄素和大黄酚分别在进样量为0.0508～0.2540μg和0.1419～0.7095μg范围内与峰面积呈线性关系;平均回收率分别为98.71%(RSD=1.37%)和98.52%(RSD=1.31%);含量分别为12.1856 mg/g和19.5257 mg/g。该方法结果准确,重现性好,可作为该方质量控制的定量方法之一。     

盐酸克林霉素阴道泡腾片的质量标准研究

采用高效液相色谱法测定盐酸克林霉素阴道泡腾片的含量方法,色谱柱为Diamonsil C18柱(250 mm×4.6 mm,5μm),检测波长214 nm,0.20 mol/L磷酸二氢铵溶液(以磷酸调节pH=3.0)-甲醇(80∶50)为流动相。流速1.0 mL/min。结果表明,在51.0~408.0μg/mL范围内,线性良好,平均回收率为90.83%,RSD为0.80%(n=6)。该法操作简便,结果准确,灵敏度高,重现性好,可用于盐酸克林霉素阴道泡腾片的质量控制。     

烫伤宁制剂质量标准的研究

建立烫伤宁制剂的质量控制标准。方法:薄层色谱法对烫伤宁制剂中的虎进行定性鉴别;采用高效液相色谱方法测定虎杖中大黄素含量。色谱柱:Hypersil ODS C18柱(250mm×4.6mm,5μm),流动相为甲醇-0.2%磷酸溶液(85:15),检测波长为254nm,流速1.0m L·min-1,柱温30℃。结果:薄层色谱斑点清晰,阴性对照无干扰;大黄素进样量在0.14~2.24μg之间呈良好的线性关系(r=0.9999),平均加样回收率为99.73%,RSD为1.59%(n=9)。结论:所建方法简单、稳定、重复性好,可用于烫伤宁制剂的质量控制。     

R-HPLC法测定鬼臼毒素软膏含量和有关物质的研究

目的:采用反相高效液相色谱法测定鬼臼毒素软膏的含量及其有关物质。方法:采用ODS C18色谱柱(5μm,4.6mm×200mm),以甲醇-水(55∶45)为流动相,流速1.0mL·min-1,检测波长292nm。结果:反相高效液相色谱法测定的线性范围为0.303~0.707mg/mL,相关系数r=0.9998;三种不同浓度供试液精密度分别为1.05%(n=5)、0.87%(n=5)、1.16%(n=5)。结论:采用反相高效液相色谱法测定鬼臼毒素软膏的含量及有关物质,方法简便、快速、准确、专属性好。     

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。     

3-甲基-4-硝基-5-氯吡唑的HPLC测定法

目的:采用高效液相色谱法测定3-甲基-4-硝基-5-氯吡唑含量.方法:用Waters symmetryC8(3.9mm×150mm,5μm)色谱柱,流动相为乙腈-0.1%磷酸溶液(50:50),流速1mL/min,柱温:25℃,检测波长274nm.结果:在160.48μg/mL～401.20μg/mL范围成线性(r=0.9998,n=5),平均回收率为98.93%,RSD=1.91%.     

HP LC法测定原料药磷酸芦可替尼的含量和有关物质

采用高效液相色谱法测定原料药磷酸芦可替尼的有关物质。以十八烷基硅烷键合硅胶柱(Inertsil ODS-3 250 L×4.6 mm,5μm)为色谱柱,甲醇:水=60:40为流动相,梯度洗脱,流速1.0 mL·min~(-1),检测波长为220 nm。结果表明,高效液相色谱法测定磷酸芦可替尼线性范围为0.518～5.175μg/mL,检测限为0.207μg/mL,定量限为0.518μg/mL,精密度(RSD=0.96%)良好,各杂质平均回收率均在90%～110%之间。高效液相色谱法测定磷酸芦可替尼的有关物质准确、有效、灵敏度高。     

高效液相色谱法测定维生素C泡腾片有关物质含量

目的:建立维生素C泡腾片中有关物质含量的测定方法。方法:采用高效液相色谱法,色谱柱为PerfectChrom 100 C18(250 mm×4.6 mm,5μm);流动相为磷酸盐缓冲溶液(pH2.50±0.05);流速:0.8mL/min;进样量:20μL;检测波长为245 nm。结果:维生素C质量浓度在4.0~16.0μg/mL范围内,进样量在0.0618~0.5562μg范围内与峰面积线性关系良好(r=0.9990)。结论:该方法简便准确,稳定性好,可用于维生素C泡腾片中有关物质的含量测定。     

甘草中甘草酸的含量测定方法研究

以高效液相色谱法检测甘草中甘草酸的含量。方法:色谱柱为C18(150 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸(38∶62),检测波长为252 nm,流速为1.0 mL·min~(-1),柱温为室温。结果:甘草酸在50～350μg/mL浓度范围内与峰面积呈良好的线性相关性(r2=0.99993);平均回收率为100.41%,RSD为0.57%(n=9),准确度良好。该方法简便、准确、可靠,适用于测定甘草及其制剂产品中的甘草酸含量。     

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。