侧柏叶黄酮的大孔树脂纯化工艺研究

为研究大孔树脂分离纯化侧柏叶黄酮提取物的最佳工艺条件,通过静态试验筛选适宜的树脂型号分离侧柏叶黄酮后,采用动态试验分别考察上样浓度、上样液pH值、上样流速与体积、洗脱液体积分数及洗脱流速对侧柏叶黄酮吸附、解吸性能的影响。结果表明,AB-8型树脂适宜分离纯化侧柏叶黄酮粗提物,最佳纯化工艺条件为：pH值为6、3mg·m L-1上样溶液60m L,以2.0m L·min-1流速上样后,采用体积分数为70%乙醇溶液140m L,以1.0m L·min-1流速洗脱,纯化后样品的黄酮纯度由（24.7±0.8）%提高至（68.2±1.1）%,表明该纯化工艺分离效果可靠,可用于侧柏叶黄酮的富集。     

毛细管电泳法测定动物肝脏中的谷胱甘肽

建立了以0.07 mol·L-1Na2HPO4-0.07 mol·L-1 KH2PO4的混合体系(pH7.38)为运行缓冲液,在230 nm紫外检测波长下,用毛细管电泳法测定鸡和猪肝脏中谷胱甘肽(GSH)的含量.结果表明:在最佳电泳条件下, GSH在5.0×10-6~1.0×10-3mol·L-1的范围内有良好的线性关系,r=0.9997,最低检出限为1.6×10-6 mol·L-1;加标回收率在94.81%~99.02%之间,RSD在1.56%~3.25%之间;该方法操作简便,快速,可靠性高,可用于动物肝脏中的谷胱甘肽含量的测定.     

聚酰胺树脂纯化荷叶碱的工艺研究

探讨了聚酰胺树脂对荷叶碱的吸附和洗脱工艺.以紫外可见分光光度法为检测手段,通过静态吸附实验考察了pH值、吸附时间对吸附量的影响,通过动态吸附实验考察了荷叶碱浓度、流速对动态泄漏点的影响,以及洗脱剂浓度、洗脱流速对洗脱率的影响.结果表明,在pH值为4、吸附时间为80 min时,聚酰胺树脂对荷叶碱的吸附性能最好,饱和吸附量为1.54 mg·mL-1;最佳上柱液浓度为0.617 mg·mL-1,动态吸附流速为0.35 BV·h-1;用流速为1.0 BV·h-1的90%乙醇溶液洗脱树脂上吸附的荷叶碱,洗脱率达到66.8%.聚酰胺树脂廉价易得,易再生,选择性高,操作简便,吸附速度较快,用乙醇洗脱无毒副作用,适于荷叶碱的纯化.     

地黄中梓醇的超声提取-树脂分离纯化工艺

研究了地黄中梓醇的超声提取-树脂分离纯化工艺。结果表明,超声提取的最佳工艺条件为：提取溶剂采用68%（体积）的乙醇,液料体积(ml)质量(g)比5:1,超声时间36 min。考察了10种大孔树脂对地黄粗提液的分离纯化效果,其中以H103对梓醇的纯化效果最佳。通过实验进一步考察了H103的动态吸附性能,得到分离纯化的最佳工艺条件为：上柱液浓度为6.15 mg·ml^-1,上柱液流速为1.0 ml·min^-1,洗脱剂为75%乙醇,洗脱流速为0.5 ml·min^-1,洗脱体积为3.33 BV（bed volume）。提取、纯化两步操作后梓醇纯度达到62.39％。     

双水相分离提取胃蛋白酶和琼脂糖的初步研究

以聚乙二醇/硫酸钠双水相体系分离提取琼脂糖和胃蛋白酶.结果表明:琼脂糖的回收率高于90%,胃蛋白酶的回收率约为50%,两者最适宜的分离条件为:pH值为3,Na2SO4浓度为0.4 g·mL-1,PEG10000的浓度为0.002 mol·L-1.     

大尺寸弱阴离子交换晶胶层析一步法分离ATP的实验研究

使用一种新型的大尺寸弱阴离子交换晶胶柱从酵母细胞发酵液中一步分离纯化广泛应用于临床治疗的高能化合物三磷酸腺苷(ATP)。该晶胶柱高150mm,直径140mm,柱体体积达到2300mL。实验测定了晶胶柱的孔隙率和等板高度等基本性能参数。层析过程以去离子水为冲洗液,分别用0.03、0.4和1mol·L-1NaCl溶液在2cm·min-1流速下进行洗脱。发现0.03mol·L-1NaCl溶液能把大部分杂质洗脱,0.4mol·L-1NaCl溶液洗脱后能获得纯度较高的ATP。洗脱下来的ATP样品通过高效液相色谱(HPLC)定量分析,回收的ATP纯度达95%～97%,总回收率49.1%。与其它已有方法相比,本法耗时少,工艺简单,降低了ATP变性的风险;在层析过程中以去离子水代替酸液作为冲洗剂和洗脱液溶剂,降低分离过程成本。     

大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺研究

优选大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺。以总皂苷的洗脱率为考察指标,通过单因素实验对大孔树脂型号、上样液浓度、吸附流速、上样量、洗脱浓度、洗脱流速、洗脱体积、氧化铝用量等因素进行考察,优选分离纯化三七总皂苷的最佳工艺条件。以D101大孔树脂纯化效果最好,最佳上样液浓度为0.5 g生药/mL,上样流速为2 BV/h(BV为柱体积),上样量(药材量∶树脂)为1∶1,依次用水、30%乙醇除杂,用量为3 BV,洗脱流速为2 BV/h,80%乙醇5 BV洗脱,收集洗脱液,将洗脱液过氧化铝柱吸附除杂,氧化铝用量为0.5 g生药/g,中试放大实验平行3次,总皂苷的纯度分别为85.96%,84.53%,86.32%,RSD值为1.13%,出膏率分别为6.45%,6.57%,6.32%,RSD值为1.94%,优选的纯化工艺稳定可行,适用于工业生产。     

大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺研究

优选大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺。以总皂苷的洗脱率为考察指标,通过单因素实验对大孔树脂型号、上样液浓度、吸附流速、上样量、洗脱浓度、洗脱流速、洗脱体积、氧化铝用量等因素进行考察,优选分离纯化三七总皂苷的最佳工艺条件。以D101大孔树脂纯化效果最好,最佳上样液浓度为0.5 g生药/mL,上样流速为2 BV/h(BV为柱体积),上样量(药材量∶树脂)为1∶1,依次用水、30%乙醇除杂,用量为3 BV,洗脱流速为2 BV/h,80%乙醇5 BV洗脱,收集洗脱液,将洗脱液过氧化铝柱吸附除杂,氧化铝用量为0.5 g生药/g,中试放大实验平行3次,总皂苷的纯度分别为85.96%,84.53%,86.32%,RSD值为1.13%,出膏率分别为6.45%,6.57%,6.32%,RSD值为1.94%,优选的纯化工艺稳定可行,适用于工业生产。     

大孔树脂分离纯化核桃青皮总黄酮的研究

以总黄酮回收率为考察指标,研究了大孔树脂分离纯化核桃青皮总黄酮的工艺。结果表明:D101型树脂对核桃青皮总黄酮有较好的吸附分离性能,是分离纯化核桃青皮总黄酮的适宜大孔树脂;最佳工艺条件为:上柱总黄酮与干树脂质量比为1:12,上样液质量浓度可在3.0875～6.175 g/L 范围内,pH值为5, 6BV(1BV=23.7 mL)的水洗后用5BV的70%乙醇洗脱。经D101处理后的核桃青皮总黄酮回收率在60%,纯度可达80%以上。该工艺简便,能有效分离纯化核桃青皮黄酮类化合物。     

粪产碱杆菌D-氨基酰化酶的分离纯化及发酵条件优化

采用热激法将含粪产碱杆菌D-氨基酰化酶基因载体的质粒导入大肠杆菌,筛选重组子,对该工程菌产生的D-氨基酰化酶用Ni 2+柱进行分离纯化;通过单因素实验优化D-氨基酰化酶的发酵条件。结果表明,纯化后的D-氨基酰化酶比活力为456.71U·mg-1,纯化回收率为50%,纯化倍数为12.4倍;最佳发酵条件为:37℃通气培养至菌体浓度OD600值为0.6时,加入0.5mmol·L-1诱导剂IPTG诱导5h,在此条件下,D-氨基酰化酶酶活力为90.9U·mL-1。     

Many Drugs of Abuse May Be Acutely Transformed to Dopamine,Norepinephrine and Epinephrine In Vivo

It is well established that a wide range of drugs of abuse acutely boost the signaling of the sympathetic nervous system and the hypothalamic–pituitary–adrenal (HPA) axis, where norepinephrine and epinephrine are major output molecules. This stimulatory effect is accompanied by such symptoms as elevated heart rate and blood pressure, more rapid breathing, increased body temperature and sweating, and pupillary dilation, as well as the intoxicating or euphoric subjective properties of the drug. While many drugs of abuse are thought to achieve their intoxicating effects by modulating the monoaminergic neurotransmitter systems (i.e., serotonin, norepinephrine, dopamine) by binding to these receptors or otherwise affecting their synaptic signaling, this paper puts forth the hypothesis that many of these drugs are actually acutely converted to catecholamines (dopamine, norepinephrine, epinephrine) in vivo, in addition to transformation to their known metabolites. In this manner, a range of stimulants, opioids, and psychedelics (as well as alcohol) may partially achieve their intoxicating properties, as well as side effects, due to this putative transformation to catecholamines. If this hypothesis is correct, it would alter our understanding of the basic biosynthetic pathways for generating these important signaling molecules, while also modifying our view of the neural substrates underlying substance abuse and dependence, including psychological stress-induced relapse. Importantly, there is a direct way to test the overarching hypothesis: administer (either centrally or peripherally) stable isotope versions of these drugs to model organisms such as rodents (or even to humans) and then use liquid chromatography-mass spectrometry to determine if the labeled drug is converted to labeled catecholamines in brain, blood plasma, or urine samples.     

Sapindaceae,cyanolipids, and bugs

Scentless plant bugs (Heteroptera: Rhopalidae) are so named because adults of the Serinethinae have vestigial metathoracic scent glands. Serinethines are seed predators of Sapindales, especially Sapindaceae that produce toxic cyanolipids. In two serinethine species whose ranges extend into the southern United States,Jadera haematoloma andJ. sanguinolenta, sequestration of host cyanolipids as glucosides renders these gregarious, aposematic insects unpalatable to a variety of predators. The blood glucoside profile and cyanogenesis ofJadera varies depending on the cyanolipid chemistry of hosts, and adults and larvae fed golden rain tree seeds (Koelreuteria paniculata) excrete the volatile lactone, 4-methyl-2(5H)-furanone, to which they are attracted.Jadera fed balloon vine seeds (Cardiospermum spp.) do not excrete the attractive lactone. Loss of the usual heteropteran defensive glands in serinethines may have coevolved with host specificity on toxic plants, and the orientation ofJadera to a volatile excretory product could be an adaptive response to save time.Mention of a commercial product does not consititute an endorsement by the USDA.     

2008～2009年世界塑料工业进展

收集了2008年7月～2009年6月世界塑料工业的相关资料,介绍了2008～2009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、环氧树脂、不饱和聚酯树脂)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。     

ICP-MS法测定地球化学样品中As、Cr、Ge、V等18种微量痕量元素的研究

建立了测定地球化学样品中包括As、Cr、Ge、V等18种微量、痕量元素的ICP-MS方法。地化试样用HF-HNO3混酸分解后,以1 1 HNO3溶解干渣。由于制样不使用盐酸,避免了Cl对As、Cr、Ge、V的质谱干扰。用国家一级地球化学标准物质GBW 07309制备溶液优化仪器工作参数,并用于校准。方法测定限(6s)为:0.007~6.4μg/g,精密度(RSD%,n=12)为:29%~9.4%,经过国家一级地球化学标准物质的分析验证,结果与标准值吻合。方法已应用于国土资源调查的试样分析。     

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.     

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.     

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.