高效液相色谱法测定阿苯达唑原料药的含量

为建立一种阿苯达唑原料药含量测定的高效液相方法,采用方法:色谱条件:Agilent ODS C18(5μm,3.0×150mm)色谱柱;以甲醇为流动相A;磷酸二氢钠水溶液(11g→800ml)为流动相B,甲醇—磷酸二氢钠水溶液=65:35时,流速为0.8ml/min,阿苯达唑对照品主峰保留时间为3.044min;分离度良好,扫描波长为292nm,柱温:30℃,结果阿苯达唑原料及溶剂峰均得到良好分离。阿苯达唑在2μg/ml¹200μg/ml浓度范围内线性良好(R2=0.99999,n=6),平均回收率98.0%,RSD为0.5%,定量限为0.1μg/ml,并得出结论:高效液相色谱法灵敏、准确,专属性强,重现性好,可用于阿苯达唑原料药含量的测定及质量控制。     

石墨炉原子吸收法直接测定尿中锰

采用自吸背景校正法,以硝酸作基体改进剂,对尿中的痕量锰进行了测定,该法在0.1—40μg/L范围呈良好的线性关系,特征量为1.53×10-11g,回收率达98.8%—101.2%.此法简便、快速且灵敏度高.     

基于RhB修饰纳米金电极测定十二烷基苯磺酸钠

借助Au-S的作用,将L-半胱氨酸组装在纳米金电极表面上,利用罗丹明B(Rhodamine B)与L-半胱氨酸之间静电的作用,将罗丹明B间接组装于纳米金电极表面,构建罗丹明B纳米金电极。采用差分脉冲伏安法,研究十二烷基苯磺酸钠在罗丹明B纳米金电极上的电化学反应,实验结果表明,在pH为4.75的醋酸-醋酸钠缓冲液中,罗丹明B纳米金电极在0—2.0×10-6g/L范围测定十二烷基苯磺酸钠的线性较好,对十二烷基苯磺酸钠检出限为2.4×10-9g/L。     

安定对抗红藻氨酸诱发小鼠惊厥作用与脑内GABA能神经元的关系

L—谷氨酸(L—Clu)、红藻氨酸(KA)icv可诱发小鼠发作性和奔跑型惊厥,CD_(50)±95％FL分别为43±18μg/mouse,及0.043±0.010μg/mouse。在苯巴比妥钠、苯妥英钠、丙戊酸钠、硫酸镁、普萘洛尔及安定6种抗惊厥药物中,安定可特异性地对抗KA惊厥。氨氧乙酸(AOAA)25mg/kg ip或GABA 67μg/mouse icv不能降低KA CD_(98)剂量诱发的惊厥发作率;氨基脲(SCZ)110 mg/kg ip或印防已毒(PIC)2mg/kg iv对KA CD_(10)剂量诱发惊厥亦无影响。但AOAA和SCZ可分别增强或减弱安定的抗惊厥作用。     

猫尾射无菌培养物的建立

本文建立猫尾射无菌培养物过程中以种子为外植体用正交试验筛选了消毒方案和诱导其萌发的培养基方案,并用直观分析法分析其结果。试验结果表明,升汞(Hgcl_2)在消毒效率中起主要作用;试验组合中,以A3B3C2的未污染率最高,为86.4％;6—BA是诱导萌发的主要因子,其极差R值为8.0％;ZT与6—BA的搭配比例对协同效应影响明显;在诱导其萌发的试验方案中,以a2b2c2d1(6—BA为1mg/L,ZT为0.5mg/L,IBA为0.5mg/L,2,4—D为0)的组合的萌发率最高,为13.3％;但是如果采用组合a2b2cld1(6—BA为1mg/L,ZT为0.5mg/L,IBA为0.1mg/L,2,4—D为0),其诱导萌发率可进一步提高。     

塞曼石墨炉原子吸收法直接测定海水锰

本文试验了几种以石墨炉原子吸收光谱法测定海水Mn的有机基体改进剂。柠檬酸及柠檬酸三铵消除海水基体干扰的效果最好。二次蒸馏水及海水Mn的特征质量(mo)及检测限(D.L.)是一致的,表明干扰已消除。用Z3030仪器获得的m_0及D.L.值分别为3.5pg及0.078μg/L;而用Z180—80仪器获得的分别为2.6pg及0.048μg/L。回收率范围为96～105％。     

尿纤维连接蛋白在诊断膀胱移行细胞癌中的应用价值

目的:评价尿纤维连接蛋白(fibronectin,Fn)在诊断膀胱移行细胞癌中的应用价值,并界定其临床参考值。方法:采用ELISA法检测55例膀胱移行细胞癌患者、34例其他泌尿系疾病患者及29例正常人的尿Fn含量,并同时测定尿肌酐(Creatin,Cr),计算Fn/Cr比值,比较各组人群尿Fn和尿Fn/Cr比值之间的差异;分析不同肿瘤分期、分级尿Fn和尿Fn/Cr之间的差异;利用尿Fn/Cr比值与其它尿生物标志物比较它们之间的优势。结果:膀胱癌组尿Fn含量(583.4±302.5μg/L)、Fn/Cr比值(149.5±93.3mg/mol)与其他泌尿系疾病组Fn含量(209.3±125.0μg/L)、Fn/Cr比值(52.4±36.2mg/mol)以及对照组Fn含量(134.3±83.6μg/L)、Fn/Cr比值(38.2±22.7mg/mol)相比,有显著性差异(P<0.01,P<0.05)。尿Fn诊断膀胱移行细胞癌的灵敏度和特异度分别为78.2%和76.2%,尿Fn/Cr比值分别为81.8%和79.4%。另外,不同分期、分级膀胱癌患者的尿Fn含量及Fn/Cr比值也有明显差异(P<0.05)。比较后提示尿Fn/Cr比值与目前多种分子生物学指标检测膀胱肿瘤的敏感性、特异性基本相似。结论:尿Fn含量及尿Fn/Cr比值在膀胱癌的临床诊断方面有重要的价值,是诊断膀胱癌的一种较理想指标;尿Fn含量及Fn/Cr的高低与膀胱癌的分期、分级有关,可大致判断膀胱癌的浸润度和恶性度,并可用于膀胱癌的预后评估,但目前仍不能代替膀胱镜;界定其临床参考值为250μg/L(Fn)和62mg/mol(Fn/Cr)。     

流动注射偶合反应化学发光测定亚硝酸根的研究

本文将亚硝酸根在酸性介质中催化溶解氧氧化Fe~(2+)的反应与Fe~(2+)-Luminol-O_2化学发光反应相偶合,利用流动注射技术,建立了一个痕量亚硝酸根的化学发光测定新方法。该方法检出限为:8×10~(-8)g/L亚硝酸根,亚硝酸根浓度在2×10~(-7)～2×10~(-4)g/L范围内与体系化学发光强度减小量呈良好线性;RSD为2.1％(C=5×10~(-6)g/L,n=7)。方法用于水样中亚硝酸根的测定,效果满意。     

GC测定风油精中薄荷脑含量的实验教学设计

设计用GC测定风油精中薄荷脑含量的药物分析实验.用乙酸乙酯为溶剂提取样品,HP25毛细管柱(530μm X 30 m,1μm)及氢火焰离子化检测器;载气为高纯氮,栽气流速2 mL/min,进样口和检测器温度均为250 ℃.标准曲线方程为A=0.008C-0.0286(R2=0.9999,n=5),在0.375～6g/L线性关系良好.高(6g/L)、中(1.5g/L)、低(0.375g/L)3个浓度的日内、日间变异均＜3%;3个浓度的加样回收率依次为99.10%、104.52%、97.30%;最低检测浓度为0.25g/L.筛选出了合适的处理样品的溶剂和最佳的GC分离条件,考查了方法的精密度和回收率,最终确定了稳定的实验条件.     

两种血清肌酐测定方法的评价

目的:对目前临床实验室测定血清肌酐较常用的肌氨酸氧化酶法和苦味酸速率法进行评价.方法:将两种测定方法进行比较,并分析各自的精密度,准确度,线性范围和干扰因素.结果:两种方法测定结果的差异无显著性(P>0.05).有良好的相关性(r=0.9905);酶法批内及日间cV分别为3.08%和3.53%,回收率为99.1%,线性范围为30-8840 umo/L;苦味酸速率法批内及日间CV分别为3.35%和3.93%,回收率为104.7%,线性范围为30-884 umol/L;884umoL/L的胆红素和10g/L的血红蛋白对酶法测定肌酐均无显著性干扰(P>0.05);10g/L的血红蛋白对苦味酸速率法测定肌酐无显著性干扰(P>0.05),但884 umoL/L的胆红素则有极显著的负干扰(P<0.01).结论:酶法是继苦味酸速率法后方法学上的又一大进步,建议使用酶法代替苦味酸速率法测定血清中的肌酐含量.     

Effect of CO2 enrichment on the glucosinolate contents under different nitrogen levels in bolting stem of Chinese kale (Brassica alboglabra L.)

The effects of CO2 enrichment on the growth and glucosinolate (GS) concentrations in the bolting stem of Chinese kale (Brassioa alboglabra L.) treated with three nitrogen (N) concentrations (5, 10, and 20 mmol/L) were investigated. Height,stem thickness, and dry weights of the total aerial parts, bolting stems, and roots, as well as the root to shoot ratio, significantly increased as CO2 concentration was elevated from 350 to 800 μl/L at each N concentration. In the edible part of the bolting stem,11 individual GSs were identified, including 7 aliphatic and 4 indolyl GSs. GS concentration was affected by the elevated CO2 concentration, N concentration, and CO2×N interaction. At 5 and 10 mmol N/L, the concentrations of aliphatic GSs and total GSs significantly increased, whereas those of indolyl GSs were not affected, by elevated atmospheric CO2. However, at 20 mmol N/L,elevated CO2 had no significant effects on the concentrations of total GSs and total indolyl GSs, but the concentrations of total aliphatic GSs significantly increased. Moreover, the bolting stem carbon (C) content increased, whereas the N and sulfur (S) contents decreased under elevated CO2 concentration in the three N treatments, resulting in changes in the C/N and N/S ratios.Also the C/N ratio is not a reliable predictor of change of GS concentration, while the changes in N and S contents and the N/S ratio at the elevated CO2 concentration may influence the GS concentration in Chinese kale bolting stems. The results demonstrate that high nitrogen supply is beneficial for the growth of Chinese kale, but not for the GS concentration in bolting stems, under elevated CO2 condition.     

Fluid components in accessory minerals of Pan-African granitoids in the Sor Rondane Mountains, East Antarctica

Fluids (fluorine, chlorine, and OH) in accessory minerals (apatite, titanite and allanite) of Pan-African granitoids(Group-Ⅰ granitoids, Group-Ⅱ granitoids and Mefjell Plutonic Complex) from the Sor Rondane Mountains, East Antarctica were precisely measured by an electronic microprobe analyzer in this study. Apatites in the granites have commonly high fluorine contents. However, fluorine contents from the Group-Ⅰ, Group-Ⅱ granitoids and Mefjell Plutonic Complex (MPC) are of important variation, which F contents (3.21～7.20 wt%) in apatite from the Group-Ⅱ granitoids are much higher than those from the Group-Ⅰ granitoids (1.22～3.60 wt%) and the MPC (3.21～4.11 wt%). Titanite in the MPC has a low fluorine content (0.23～0.50 wt%), being less than those in the Group-Ⅰ granitoids (2.28 wt%) and Group-Ⅱ granitoids (1.85～2.78 wt%). Fluorine in allanite in the Group-Ⅱ granitoids seems to have much lower contents than those from the Group-Ⅰ granitoids and the MPC. Higher fluorine contents in the titanite from the Group-Ⅱ granitoids may be mainly controlled by late-magmatic fluid-rock interaction processes associated with melt, but may not be indicative of original magma contents based on its petrographic feature. Due to very lower chlorine contents from all of accessory minerals, the authors suggest that titanite and apatite with higher fluorine contents in the Group-Ⅱ granitoids have much lower H2O (OH) contents compared with those in the Group-Ⅰ granitoids according to the partition among (F, Cl, OH).Fluorine contents in whole-rock samples show a variation from the higher in the Group-Ⅰ granitoids to the lower in the Group-Ⅱ granitoids and the MPC, which are consistent with the changes of those from the biotite and hornblende as well as fluorite occurred in the Group-Ⅰ granitoids reported previously. Based on the above study of fluorine in accessory minerals and combined with the previous fluorine contents from biotites and hornblendes, the authors suggest that apatites and titanites with higher F contents in the Group-Ⅱ granitoids and the MPC may not be an indicator of higher fluorine contents in whole-rock, which reflect fluorine contents in magma sources and/or late-thermal activity. Higher fluorine contents in apatite, titanite and allanite may be an additional evidence of A-type affinity.     

Fluid components in accessory minerals of Pan-African granitoids in the S■r Rondane Mountains, East Antarctica

Fluids (fluorine, chlorine, and OH) in accessory minerals (apatite, titanite and allanite) of Pan-African granitoids (Group-I granitoids, Group-II granitoids and Mefjell Plutonic Complex) from the S?r Rondane Mountains, East Antarctica were precisely measured by an electronic microprobe analyzer in this study. Apatites in the granites have commonly high fluorine contents. However, fluorine contents from the Group-I, Group-II granitoids and Mefjell Plutonic Complex (MPC) are of important variation, which F contents (3.21~7.20 wt%) in apatite from the Group-II granitoids are much higher than those from the Group-I granitoids (1.22~3.60 wt%) and the MPC (3.21~4.11 wt%). Titanite in the MPC has a low fluorine content (0.23~0.50 wt%), being less than those in the Group-I granitoids (2.28 wt%) and Group-II granitoids (1.85~2.78 wt%). Fluorine in allanite in the Group-II granitoids seems to have much lower contents than those from the Group-I granitoids and the MPC. Higher fluorine contents in the titanite from the Group-II granitoids may be mainly controlled by late-magmatic fluid-rock interaction processes associated with melt, but may not be indicative of original magma contents based on its petrographic feature. Due to very lower chlorine contents from all of accessory minerals, the authors suggest that titanite and apatite with higher fluorine contents in the Group-II granitoids have much lower H2O (OH) contents compared with those in the Group-I granitoids according to the partition among (F, Cl, OH). Fluorine contents in whole-rock samples show a variation from the higher in the Group-I granitoids to the lower in the Group-II granitoids and the MPC, which are consistent with the changes of those from the biotite and hornblende as well as fluorite occurred in the Group-I granitoids reported previously. Based on the above study of fluorine in accessory minerals and combined with the previous fluorine contents from biotites and hornblendes, the authors suggest that apatites and titanites with higher F contents in the Group-II granitoids and the MPC may not be an indicator of higher fluorine contents in whole-rock, which reflect fluorine contents in magma sources and/or late-thermal activity. Higher fluorine contents in apatite, titanite and allanite may be an additional evidence of A-type affinity.     

Effect of CO2 enrichment on the glucosinolate contents under different nitrogen levels in bolting stem of Chinese kale (Brassica alboglabra L.)

The effects of CO₂ enrichment on the growth and glucosinolate (GS) concentrations in the bolting stem of Chinese kale (Brassica alboglabra L.) treated with three nitrogen (N) concentrations (5, 10, and 20 mmol/L) were investigated. Height, stem thickness, and dry weights of the total aerial parts, bolting stems, and roots, as well as the root to shoot ratio, significantly increased as CO₂ concentration was elevated from 350 to 800 μl/L at each N concentration. In the edible part of the bolting stem, 11 individual GSs were identified, including 7 aliphatic and 4 indolyl GSs. GS concentration was affected by the elevated CO₂ concentration, N concentration, and CO₂×N interaction. At 5 and 10 mmol N/L, the concentrations of aliphatic GSs and total GSs significantly increased, whereas those of indolyl GSs were not affected, by elevated atmospheric CO₂. However, at 20 mmol N/L, elevated CO₂ had no significant effects on the concentrations of total GSs and total indolyl GSs, but the concentrations of total aliphatic GSs significantly increased. Moreover, the bolting stem carbon (C) content increased, whereas the N and sulfur (S) contents decreased under elevated CO₂ concentration in the three N treatments, resulting in changes in the C/N and N/S ratios. Also the C/N ratio is not a reliable predictor of change of GS concentration, while the changes in N and S contents and the N/S ratio at the elevated CO₂ concentration may influence the GS concentration in Chinese kale bolting stems. The results demonstrate that high nitrogen supply is beneficial for the growth of Chinese kale, but not for the GS concentration in bolting stems, under elevated CO₂ condition. Project (No. 2007CB109305) supported by the National Basic Research Program (973) of China     

Effect of NaCl treatments on glucosinolate metabolism in broccoli sprouts

To understand the regulation mechanism of NaCl on glucosinolate metabolism in broccoli sprouts,the germination rate,fresh weight,contents of glucosinolates and sulforaphane,as well as myrosinase activity of broccoli sprouts germinated under 0,20,40,60,80,and 100 mmol/L of NaCl were investigated in our experiment.The results showed that glucoerucin,glucobrassicin,and 4-hydroxy glucobrassicin in 7-d-old broccoli sprouts were significantly enhanced and the activity of myrosinase was inhibited by 100 mmol/L of NaCl.However,the total glucosinolate content in 7-d-old broccoli sprouts was markedly decreased although the fresh weight was significantly increased after treatment with NaCl at relatively low concentrations(20,40,and 60 mmol/L).NaCl treatment at the concentration of 60 mmol/L for 5 d maintained higher biomass and comparatively higher content of glucosinolates in sprouts of broccoli with decreased myrosinase activity.A relatively high level of NaCl treatment(100 mmol/L) significantly increased the content of sulforaphane in 7-d-old broccoli sprouts compared with the control.These results indicate that broccoli sprouts grown under a suitable concentration of NaCl could be desirable for human nutrition.     

Changes in biochemical constituents and induction of early sprouting by triadimefon treatment in white yam （Dioscorea rotundata Poir.） tubers during storage

The ability of triadimefon(TDM),a triazolic fungicide,to alter the biochemical constituents and thereby minimizing the days required for sprouting in white yam(Dioscorea rotundata Poir.) tubers during storage under(30±2) °C in the dark,was studied.TDM at 20 mg/L was given to tubers by dipping the tubers in treatment solution containing 20 mg/L TDM on 10,25 and 40 d after storage(DAS).Starch,sugars,protein,amino acid contents as well as protease and α-amylase activities were estimated on 15,30 and 45 DAS from two physiological regions viz.,apical and basal regions of the tubers.In normal conditions(control) sprouting occurred on 70 to 80 DAS.The starch content decreased,while protein,amino acid,sugar contents and protease and α-amylase activities were increased due to TDM treatment and led to early sprouting.     

碱提取法从虎杖中分离白藜芦醇的方法研究

实验对白藜芦醇采用无机碱性水溶液进行提取、然后选择适宜的pH值进行沉降,完成对白藜芦醇的分离.采用单因素实验,对原料粒度、无机碱的种类及用量、酸的用量、浸泡时间等因素进行探究,确定了碱提取酸沉淀方法分离白藜芦醇的最佳条件:原料粒度为过40目筛;提取溶剂为氢氧化钾调节蒸馏水pH值为10;浸泡时间为12 h;恒速、均匀搅拌,加热煮沸1 h;抽虑,沉淀试剂为1 mol/L的盐酸调节pH值为3,静置充分沉淀.所得到的粗提物经过紫外、红外光谱检测,确实含有白藜芦醇.表明碱提取酸沉淀的分离方法工艺简单,操作安全,是行之有效的分离方法.     

NaCl胁迫对青稞幼苗部分生理指标的影响

以青稞幼苗为试材,采用营养液水培法研究了200mmol／L NaCl胁迫对青稞幼苗叶片相对含水量（RWC）、叶绿素、丙二醛（MDA）、脯氨酸含量的影响．结果显示,在200mmol／L NaCl胁迫2,4,6,8d后,青稞幼苗叶片相对含水量、叶绿素含量随胁迫的进行而不断下降,其中叶绿素含量在前4d下降尤其明显;MDA和脯氨酸含量则显著上升．表明200mmol／L NaCl胁迫对青稞幼苗造成了严重的生理伤害．     

Vacuum pyrolysis characteristics of waste epoxy printed circuit boards

Vacuum pyrolysis was employed to dispose scrap brominated epoxy printed circuit boards (PCBs). Pyrolysis characteristics of waste PCBs under normal pressure and vacuum were investigated in this paper. A detailed study on the analysis of the elemental composition of PCBs and the pyrolysis products was performed. The thermal decomposition kinetics was measured by a thermogravimetric (TG) analyzer. The activation energy of pyrolysis under nitrogen atmosphere and vacuum were 193 kJ/mol to 206 kJ/mol and 145 kJ/mol to 165 kJ/mol, respectively. The composition of materials was analyzed by elemental analyzer. The pyrolysis products were analyzed by GC (gas chromatograph), GC-MS (chromatography and mass spectrometry) and FT-IR (Fourier transform infrared spectroscopy). Vacuum helped to increase the yield of pyrolysis oil. The liquid yield of PCBs pyrolysis at 15 kPa and normal pressure were 31.3? and 23.5?, respectively. The main components in pyrolysis oils were phenol, isopropyl-phenol, and their brominated substitution.     

NaCl胁迫对油菜幼苗膜脂过氧化和抗氧化酶活性的影响

为研究NaCl胁迫对油菜幼苗膜脂过氧化和抗氧化酶活性的影响,用不同浓度的NaCl溶液分别对油菜幼苗进行胁迫,在不同的时间分别对油菜幼苗MDA含量,以及SOD、CAT活性进行测定.研究结果表明:100mmol/L浓度以下油菜幼苗MDA含量稍有降低,但是随着NaCl胁迫浓度的升高和胁迫时间的延长,油菜幼苗MDA含量均升高.100mmol/L浓度以下,随着胁迫时间的延长油菜幼苗的CAT和SOD酶活性均上升,高盐胁迫下(200mmol/L以上),随着胁迫浓度和胁迫时间的延长,CAT和SOD活性均先升高后降低.这说明油菜幼苗对NaCl胁迫存在浓度依赖和时间依赖关系.