荆芥挥发油成分的气相色谱-质谱分析

目的定性、定量分析荆芥挥发油成分.方法采用气相色谱-质谱检测,通过化学计量学解析法对二维色谱/质谱数据进行解析,得到各组分的纯色谱曲线和质谱,从而实现对荆芥挥发油成分的定性、定量分析.结果鉴定了51个荆芥挥发油成分,占挥发油成分总含量的86.71%. 结论荆芥挥发油主要组分为D-薄荷酮 （22.22%）, 4-甲氧基-3-甲基-1,2-苯二胺（14.38%）, 薄荷酮（4.44%）, 2-辛醛（4.03%）,（2R-反）-5-甲基-2-（1-甲基乙烯基）环己酮（3.28%）, 2-异亚丙基-5-甲基环己酮（1.76%）, 4,11,11-三甲基-8-亚甲基二环[7.2.0]- 4-壬烯（1.32%）, 1-辛烯-3-醇（1.28%）.     

药对麻黄-葛根挥发油成分分析

目的定性定量分析药对麻黄-葛根、麻黄、葛根的挥发油成分.方法采用气相色谱-质谱(GC-MS)检测,通过化学计量学解析法对二维色谱/质谱数据进行解析.结果麻黄-葛根、麻黄和葛根挥发油成分分别定性得到57、70和33个结果,占总含量的93.17%、89.52%和88.84%.结论药对挥发油成分的数目大致为麻黄和葛根挥发油成分的加和.     

金银藤挥发油成分的气-质联用分析与化学计量学解析

目的 定性、定量分析金银藤挥发油成分.方法 采用气相色谱-质谱进行检测,通过化学计量学解析法对二雏色谱/质谱数据进行解析,得到各组分的纯色谱曲线和质谱,从而实现对金银藤挥发油成分的定性、定量分析,并结合程序升温保留指数来鉴定化合物.结果 金银藤的挥发油鉴定了39个成分,定性组分含量占金银藤挥发油成分总含量的94.54%.结论 全银藤挥发油的主要成分为十六烷酸（45.86%）、9,12-十八碳二烯政乙酯（39.02%）、十四烷酸（1.8%）、十五烷酸（1.07%）、十八烷酸（1.02%）.     

食品中苏丹红检测研究进展

本文评述了高效液相色谱（HPLC）、液相色谱-质谱（LC／MS）、气相色谱-质谱（GC／MS）以及薄层色谱法（TLC）对食品中苏丹红的检测研究进展，内容着重包括苏丹红样品预处理、净化，色谱检测波长的选择、流动相的选择、色谱检测器的选择，薄板及展开剂的选择等。     

应用循环式液—液萃取法分离及鉴定木素生物降解物质

紫外光谱分析结果表明循环式液－液萃取器可有效抽提富集微量木素生物降解物质，抽提物通过气相色谱－质谱联用仪鉴定出４０余种木素生物降解相关物质组分，不同结构木素经不同酶处理后期降解产物组成及含量有显著差异，为木素生物降解机制研究了一种新方法。     

毒死蜱完全抗原的合成与表征

在碱性条件下将毒死蜱原药与3-巯基丙酸反应,得到毒死蜱半抗原(O,O二乙基-O-[3,5一二氯-6-(2-羧乙基)硫代-2-吡啶基]硫代磷酸酯),采用活泼酯法将生成的半抗原与牛血清白蛋白(BSA)偶联,制备完全抗原.红外光谱、气相色谱-质谱联用仪及紫外光谱测试结果表明,所合成的物质均为目标产物.本方法简便易行,为利用免疫传感器快速检测有机磷农药毒死蜱残留量解决了一个关键技术问题.     

食品中胺鲜酯的气相色谱-质谱联用仪测定方法研究

为检测食品中胺鲜酯残留量,以大米、白菜、玉米为研究对象,建立了食品中胺鲜酯的气相色谱-质谱联用仪测定方法。样品经丙酮微波萃取,固相萃取柱净化,氮吹浓缩,用气相色谱-质谱联用仪测定,外标法定量。结果表明:胺鲜酯在20~4000 ng/L范围内具有良好的线性关系(R=0.9999),方法检出限6μg/kg,定量限20μg/kg。在40~4000μg/kg的添加水平,胺鲜酯的回收率在95%~107%之间,方法精密度试验的相对标准偏差在5%以内。该方法适用于食品中胺鲜酯的定性和定量测定。     

测定肿瘤细胞内外5-氟尿嘧啶含量的方法研究

目的建立了高效液相色谱法测定A549组胞内外5-氟尿嘧啶含量的方法,为探索5-氟尿嘧啶的作用机理奠定基础。方法色谱柱采用Hypersil ODS柱（4．6mm×250mm,5μm）;流动相为甲醇·水=2：98（V／V）;流速：0．8ml／min;柱温：30℃;检测波长：265nm;进样量为5μl。结果细胞内液中5-氟尿嘧啶在0.1～50．0μg/ml范围内线性关系良好（r=0．9996）,平均回收率为97．65％,RSD为0．40％,日内和日间精密度分别为1．30％,1．04％;细胞跨液中5-氟尿嘧啶在1．0～250．0μg/ml范围内线性关系良好（r=0.9999）,平均回收率为102.34％,RSD为2．11％,日内和日间精密度分别为1．32％,1．06％。结论该色谱方法简便易行,准确度高,重现性好,可用于细胞内外5-氟尿嘧啶浓度的动态变化规律研究。     

柴黄颗粒中黄芩苷的含量测定研究

目的建立柴黄颗粒中黄芩苷的含量测定方法。方法采用Alltima C18（5μm,150mm×4．6mm）色谱柱;流动相为甲醇-0．3％磷酸溶液（50：50）;检测波长为280nm。结果黄芩苷峰与其他杂质峰分离良好,在0．3302-0．7706雌范围内,黄芩苷线性关系良好（r=0．9998）,平均回收率为101．05％（n=2）RSD=1．39％。结论该方法简便易行,准确度高,重现性好,可用于柴黄颗粒的质量控制。     

色谱联用技术在环境和生物样品中痕量超痕量元素形态分析研究进展

随着分析科学的不断发展,常用的元素分析方法,如光谱技术(AES,AFS)和质谱等已不能满足环境和生物样品中痕量、超痕量元素的赋存形态分析。以色谱联用技术为代表的元素形态分析测试技术(如液相色谱-原子光谱联用、色谱-电感耦合等离子质谱联用、毛细管电泳-电喷雾离子化质谱联用技术等)已成为国内外研究的热点。本文扼要的介绍了近年来国内外在环境和生物样品中痕量、超痕量元素砷、硒、汞形态分析的色谱联用技术研究进展,并侧重于样品前处理方法、痕量或超痕量元素的形态分析技术。     

Leichtflüchtige Stoffe inAgaricus bisporus

Summary The composition of the volatile fractions (isolated by acidic steam distillation) of the spores, substrate mycelium and fruiting body of the common mushroom is investigated. The physiological and/or biochemical functions of some of the identified substances are discussed.     

离子液体双水相萃取红霉素的研究

建立了由亲水性离子液体[Emim] BF4和NaH2PO4形成的双水相体系萃取红霉素的新方法.考察了磷酸盐浓度、离子液体用量、萃取温度、震荡时间、pH值、萃取次数等因素对红霉素萃取率的影响;分析了离子液体的可再生性.结果表明,在红霉素溶液中加入3.5g离子液体,调节体系pH到7～8,温度在303.15 K下,萃取时间2～3h,红霉素的萃取率为87.2％;萃取3次后,萃取率可达98.32％;离子液体重复利用可达到5次.研究表明,离子液体双水相体系可成功用于红霉素的富集分离中,为食品中微痕量红霉素的测定提供新方法.     

超临界CO2在制备PCL/水杨酸甲酯控释体系中的应用研究

本文利用超临界二氧化碳（SCCO2）对生物可降解材料--聚己内酯（PCL）进行溶胀和塑化,进而将其作为携带剂,将水杨酸甲酯嵌入到PCL中,制备含有水杨酸甲酯的PCL多孔材料,即PCL/水杨酸甲酯控释体系,并研究超临界流体条件下水杨酸甲酯的插嵌规律.研究结果表明,PCL对水杨酸甲酯有很好的吸附能力,通过测定所制备的多孔材料PCL/水杨酸甲酯体系的缓释行为,表明其多孔结构对药物分子具有一定的缓释功能,药物分子释放时间最长可达18 h以上.     

JNK1-dependent antimitotic activity of thiazolidin compounds in human non-small-cell lung and colon cancer cells

We recently identified two thiazolidin compounds, 5-[(4-methylphenyl)methylene]-2-(phenylamino)-4(5H)-thiazolone (MMPT) and 5-(2,4-dihydroxybenzylidene)-2-(phenylimino)-1,3-thiazolidin (DBPT), that inhibit the growth of human non-small-cell lung and colon cancer cells independent of P-glycoprotein and p53 status. Here we further investigated the mechanism by which these thiazolidin compounds mediate their anticancer effects. Treatment of cancer cells with MMPT and DBPT led to a time-dependent accumulation of cells arrested in the G2/M phase with modulation of the expression of proteins such as cyclin B1, cdc25C, and phosphorylated histone H3. Moreover, treatment with MMPT and DBPT increased M-phase arrest with abnormal spindle formation. DBPT-mediated G2/M phase arrest and phosphorylation of cdc25C and histone H3 were abrogated when JNK activation was blocked either with SP600125, a specific JNK inhibitor, or a dominant-negative JNK1 gene. Moreover, DBPT-mediated microtubule disruption was also blocked by SP600125 treatment. Our results demonstrate that thiazolidin compounds can effectively induce G2/M arrest in cancer cells and that this G2/M arrest requires JNK activation.     

Closing the door on Hugo de Vries' Mendelism

In the first part of the 19th century, geologists explained volcanoes, earthquakes and mountain-formation on the assumption that the earth has a large molten core underneath a very thin (25–50 mile) solid crust. This assumption was attacked on astronomical grounds by William Hopkins, who argued that the crust must be at least 800 miles thick, and on physical grounds by William Thomson, who showed that the earth as a whole behaves like a solid with high rigidity. Other participants in the debate insisted that there is evidence for a fluid or plastic layer not far below the crust. It was also suggested that the interior of the earth is a supercritical fluid. By the end of the century many geologists had incorporated the doctrine of a completely solid earth into their theories. Acceptance of a relatively small liquid core, indicated by seismological research, was delayed for another two decades.     

Triphasic vascular effects of thiol compounds and their oxidized forms on dog coronary arteries

The vascular effects of 2-mercaptoethanol, cysteamine, L-cysteine, glutathione (GSH), cystamine and oxidized GSH (GSSG) on the isometric tension of isolated dog coronary arterial strips were examined, and these effects were compared with the triphasic response induced by dithiothreitol (DTT); a rapid and weak contraction (phase A), an intervening slow relaxation (phase B) and a slowly-developing strong contraction (phase C) which we previously reported. The responses of the arteries induced by 2-mercaptoethanol, cysteamine and L-cysteine consisted of phases A, B and C. The order of contractile potency (ED₅₀ of phase C) was DTTL-cysteine>2-mercaptoethanolcysteamine, while the order of relaxant potency (ED₅₀ of phase B) was DTT>cysteamine2-mercaptoethanol. GSSG and cystamine mainly produced relaxation, which corresponded to phase B. The phase C contraction was specific to the reduced forms of thiols, except for GSH, which produced only relaxation. The participation of endothelial cells was not essential for the contracting or relaxing effects of the thiol compounds. The phase C contraction was depressed by W-7, a calmodulin antagonist, while phase A was not. Therefore calmodulin-dependent protein kinases may participate in phase C, not in phase A.     

Insecticidal effect of trans-2-nonenal,a constituent of carrot root

Summary Vapour of trans-2-nonenal killed the carrot fly larva,Psila rosae, with an LC₅₀ of 2.17 mg/24h. The aldehyde was identified in the essential oil of carrot in concentrations of up to 40 g/root.Special thanks are due to The Agricultural Institute, Dublin, for funding a proposal from M.F.R.     

Effects of CO2 exposure on distribution of various forms of iron and copper in guinea-pig tissues

The effects on iron and copper distribution and metabolism of exposure to high levels of CO2 were studied in the guinea-pig. Mature, male animals were placed in an atmosphere of 15% CO2, 21% O2 (balance N2), and sacrificed from 1 h to 1 week thereafter. Total iron and copper concentrations of blood, liver, spleen and bone, as well as concentrations of heme and ferritin iron, were measured together with blood hematocrit, reticulocytes, plasma hemoglobin, plasma ceruloplasmin and copper concentrations. The results show clearly that rapid and sustained red cell damage or hemolysis ensued several h from the start of CO2 treatment. This resulted in loss of iron and copper from the blood, an influx of both elements into liver, spleen and bone, and a rise in plasma ceruloplasmin. Influx of iron into liver and spleen caused an accumulation of ferritin, the main site for iron storage in cells. Following the effect on red cells, there was an accumulation of heme iron, and a decreased hematocrit, best explained by a depressed activity of the reticuloendothelial and erythropoietic systems. A period of adaptation succeeded these events, in which all blood parameters and most tissue values returned to normal, despite the continuing presence of high CO2. The only changes not reversed were the elevations in liver, spleen and bone iron stores. These remained high, with a net accumulation of greater than 2 mg iron, or 3-4 times more than originally present. The results indicate that at least in the guinea-pig, high CO2 exposure results in red cell damage and other events leading to an accumulation of additional iron in the body; also, that iron accumulated as ferritin and hemosiderin in liver and spleen may not be readily available to restore blood hemoglobin concentrations on an acute basis.     

分子印迹基质固相分散．液相色谱法测定水产品中的磺胺类抗生素残留

以获得的对磺胺类抗生素具有特异选择性的分子印迹聚合物作为吸附材料,建立分子印迹基质固相分散萃取技术;对水产品中的SAs进行富集、纯化,进一步结合高效液相色谱法;建立基于分子印迹技术的水产品中SAs检测的新方法。结果表明,虾和鱼样品中磺胺嘧啶、磺胺甲嘧啶、磺胺15-甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲唿唑、磺胺二甲氧嘧啶的最低检测限分别为11．8、11．1、11．4、10．8、9．8、9．4μg／kg和10．7、11．2、11．4、10．6、9．4、9．9μg／kg,最低定量限分别为27．1、31．6、28．8、27．3、29．3、28．3μg／kg和26．2、28．0、27．2、28．6、25．0、25．6μg／k,六种SAs回收率均达80％以上．可应用于水产样品中SAs的定号检测．     

Increase in Na+, K+ -ATPase enzyme units in liver and kidneys from essential fatty acid deficient rats.

(3H)-Ouabain binding to liver and kidney preparations was utilized to estimate the number of Na+, K+-ATPase enzyme units in livers and kidneys from rats fed 2% corn oil supplemented or fat-free diets. The specific (3H)-ouabain binding in liver and kidney preparations from fatty acid deficient rats was increased approximately 40%, but the affinity of the binding sites for ouabain (Kd-value) remained unchanged. The increased concentration of Na+, K+-ATPase enzyme units observed in the essential fatty acid deficient rats may contribute to the reduced body fat accumulation and elevated heat production observed in these animals.