高效液相色谱法检测化妆品中儿茶酚胺类药物的残留量

采用高效液相色谱法,研究检测了化妆品中肾上腺素、去甲肾上腺素、异丙肾上腺素的残留量.得到的色谱条件:Waters Atlantis C_(18)柱(5μm,250 mm×4.60 mm)为分析柱,流动相V(甲醇):V(0.02 mol/L磷酸二氢钾溶液)=4:96,荧光检测器检测,激发波长为285 nm,发射波长为340 nm.结果表明,肾上腺素、去甲肾上腺素在0.025 mg/L～2.5 mg/L内,异丙肾上腺素在0.05 mg/L～5.0 mg/L内,其峰面积与质量浓度呈良好的线性关系.该方法回收率为95.6%～99.4%,RSD为3.6%～6.1%(n=8).     

反相高效液相色谱法测定化妆品中的3-O-乙基维生素

采用反相高效液相色谱法测定化妆品中的3-O-乙基维生素C,色谱条件:SH IMADZU Sh im-pack VP-C18ODS(150 mm×4.6 mm,5μm)色谱柱;C18ODS保护柱芯;流动相V(甲醇)∶V(0.025 mol/L KH2PO4)=20∶80;流速:1.0 mL/m in;柱温:30℃;紫外检测器检测,检测池温度:40℃,波长:254 nm。结果表明,在此条件下,3-O-乙基维生素C在0~100 mg/L与相应的峰面积具有良好的线性关系(r=0.999 2),线性回归方程为A=31.170 3,ρ回收率在97.75%~100.60%,方法精密度RSD约为2.6%(n=5)。     

HPLC-ELSD法测定壳寡糖降解液中氨基葡萄糖盐酸盐

建立HPLC-ELSD测定壳寡糖降解液中氨基葡萄糖含量的分析方法。用单因素和正交试验对壳寡糖微波条件进行优化,确定最佳降解条件:30%盐酸,功率300 W,时间60 min,料液比1∶20。色谱条件:Prevail Carbohydrate ES柱(4.6 mm×250 mm,5μm),流动相乙腈-水(75∶25),流速1.0 m L·min~(-1)。ELSD漂移管温度:60℃;载气流量:1.5 L/min;进量样5μL,柱温30℃。氨基葡萄糖盐酸盐的质量浓度对数在0.1~0.8 mg/m L与色谱峰面积对数呈良好线性关系,相关系数为r=0.9987,回收率在83.3%~95.5%之间,相对标准偏差为3.9%(n=9)。     

HPLC法测定重组人胰高血糖素类多肽-1(7-36)注射液中苯酚含量

目的建立高效液相色谱法测定重组人胰高血糖素类多肽-1(7-36)注射液中苯酚含量的方法。方法采用C18烷基硅烷键合硅胶色谱柱(Venusil XBP-C18 5um 100A 4.6×250mm),流动相A:甲醇(HPLC),流动相B:超纯水,流速:1m L/min,柱温为25℃,进样量为10μL,波长269nm。结果精密度试验RSD为0.086%(n=6);苯酚的浓度在0.044 mg/m L-0.44 mg/m L范围内与峰面积有良好的线性关系(R20.9999);平均回收率为99.20%(n=9);不同色谱条件下,耐用性良好。结论该方法快速、简便、重复性好,适用于重组人胰高血糖素类多肽-1(7-36)注射液中苯酚含量的测定。     

高效液相色谱-蒸发光散射法测定蛇皮中胶原蛋白含量

建立高效液相色谱-蒸发光散射检测(HPLC-ELSD)法测定蛇皮胶原蛋白含量的方法。胶原蛋白经盐酸水解后,采用Thermo Hypersil Gold C18(250 mm×4.6 mm,5μm)色谱柱进行分离,以乙腈(含0.2%甲酸,A相)-0.2%甲酸水溶液(B相)为流动相进行梯度洗脱,洗脱时间15 min,柱温30℃,流速0.4 m L/min。ELSD参数:雾化器温度85℃,蒸发器温度85℃,氮气作载气,蒸发器气流1.2 L/min。进样量10μL。在此条件下,羟脯氨酸的线性范围为10~100 mg/L,R2=0.999 6,检测限为5.56 mg/L,定量限为10 mg/L。蛇皮胶原蛋白的平均回收率为94.53%,RSD为2.15%。蛇皮中胶原蛋白质量分数平均值为40.21%,为蛇皮的主要蛋白质。     

HPLC法测定牛奶中的舒巴坦

建立了反相高效液相色谱内标法测定牛奶中舒巴坦的方法。色谱条件:日本岛津C18柱(4.6mm×250mm i.d.,5μm),柱温:30℃,流动相:乙腈-磷酸盐缓冲液=8:92,p H5.0(V/V),流速:1m L/min,λs=210nm。在1.004~20.08mg/L范围内均呈良好的线性关系,线性相关系数为0.9996,内标工作曲线法定量。实验结果:舒巴坦的平均回收率为97.3%(RSD=0.41%)。结论:本法简便,快速,准确,精密,已经应用于实际样品的检测。     

紫杉醇纳米脂质载体包封率的测定

建立紫杉醇纳米脂质载体包封率测定的高效液相色谱法。选择色谱条件:Diamonsil-C18柱(200mm×4.6 mm,5μm);柱温30℃;流动相:0.067 mol/L磷酸二氢铵水溶液(三乙胺调p H为7.5)-乙腈(3∶2);检测波长205 nm;体积流量1.0 m L/min;进样量20μL。对该色谱条件下测定紫杉醇的方法学进行考察,建立超滤离心法测定紫杉醇纳米脂质载体的包封率。在此色谱条件下紫杉醇与辅料及溶剂峰均得到良好分离,紫杉醇在50.00~1000μg/m L浓度范围内线性关系良好(R=0.9995,n=7),超滤离心法测得紫杉醇纳米脂质载体的包封率为(88.7±0.2)%。该方法准确可靠、简单快速。可用于紫杉醇纳米脂质载体包封率的测定。     

双氟·唑嘧胺悬浮剂的高效液相色谱分析

采用Agilent ZORBAX Eclipse XDB-Cl8(5μm,150×4.6 mm i.d)色谱柱,以甲醇:水(醋酸0.5%)溶液(38:62,V/V)为流动相,检测波长260 nm,在同一色谱条件下测定175 g/L双氟·唑嘧胺悬浮剂中的唑嘧磺草胺和双氟磺草胺。唑嘧磺草胺变异系数为0.34%,平均回收率为100.3%;双氟磺草胺变异系数为0.42%,平均回收率为99.5%。     

高效液相色谱-二极管阵列检测法测定马来酸和乙醛酸

建立了高效液相色谱-二极管阵列法同时测定乙醛酸和马来酸的高效液相色谱方法。色谱条件为:Shim-pack VP.ODS柱(250 mm×4.6 mm I.D.,5μm);二极管阵列检测器;流动相为甲醇/磷酸盐缓冲溶液(NaH2PO4浓度为0.1 mol/L,H3PO4调节至pH=2.98),体积比为5∶95,流速为1.0 mL/min,检测波长为195 nm,柱温为40℃。线性范围分别为79.6～26 660 mg/L和9.3～7 864 mg/L,检出限分别为39.4 mg/L和4.7 mg/L;日内、日间测定的相对标准偏差(RSD):乙醛酸为0.22%和0.46%,马来酸为0.02%和0.03%。     

高效液相色谱法同时测定厚朴提取物中厚朴酚与和厚朴酚

建立了同时测定厚朴提取物中厚朴酚与和厚朴酚的高效液相色谱检测方法。采用Agilent ODS-C18(5μm,4.6 mm×250 mm)液相色谱柱,以甲醇∶水=80∶20为流动相,流速为1 mL/min,检测波长为294 nm,柱温为35℃。结果表明,厚朴酚在质量浓度4.48~224.00 mg/L,和厚朴酚在6.70~335.00 mg/L时与色谱峰面积的线性关系良好,相关系数r均为0.9995。厚朴酚与和厚朴酚平均加标回收率分别为97.83%、101.53%,峰面积相对标准偏差RSD(n=6)分别为1.15%和0.14%。该方法快速、准确,重现性好,可以对厚朴提取物中厚朴酚与和厚朴酚的进行定量分析。     

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.     

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.