大气颗粒物中总碳含量的测量不确定度评定

分析了元素分析仪测定大气颗粒物中碳质组分的测量不确定度来源,对总碳含量的测量不确定度进行了评估。测定咖啡碱标准样品中的碳含量,称样量为1 500~2 500μg时,测定结果为(49.27±0.26)%;测定大气颗粒物样品中的总碳含量,样品面积为3.14 cm2时,测定结果为(106±3)μg/cm2。     

采用纳氏试剂分光光度法监测地表水氨氮时样品预处理方法改进

采用HJ535-2009《水质氨氮的测定纳氏试试剂分光光度法》测定水样氨氮时,当水样浑浊或有颜色时用蒸馏法对样品进行预处理,但该处理方法测定结果偏低,远远超出误差允许范围。提出以0.45μm滤膜过滤样品后进行测定,并在比色过程用过滤水样作色度校准。方法改进后对标准样品进行测定,测定结果与标准值相一致。采用改进后的方法对实际样品进行测定,加标回收率为96.7%,测定结果的相对标准偏差为3.60%(n=6)。该法测试数据稳定、结果可靠,适合于汛期地表水中氨氮的测定。     

微生物传感器快速测定生化需氧量

利用微生物传感器快速测定水中生化需氧量。用该法对标准样品进行测定,测定结果的相对标准偏差为3.30%~4.67%(n=4),与标准值的相对误差在±5%之内。用该方法和经典稀释接种法对实际样品进行测定,该方法测定结果的相对误差为4.1%~11.3%。微生物传感器法能满足环境监测的要求。     

超高效液相色谱-质谱法测定肉类食品中瘦肉精的不确定度评定

评定超高效液相色谱-质谱法测定肉类食品中4种类型的瘦肉精含量的不确定度。通过计算不确定度来确定关键影响因素,优化实验方法,提高检测工作的质量。建立数学模型,对各不确定度的来源进行分析和评定。在置信概率P为95%,k=2,肉类食品中盐酸克伦特罗测定结果的扩展不确定度为0.035 2;莱克多巴胺测定结果的扩展不确定度为0.037 8;特布他林测定结果的扩展不确定度为0.082 8;沙丁胺醇测定结果的扩展不确定度为0.027 6。盐酸克伦特罗测定结果的不确定度主要来源于重复测量和标准物质的浓度;莱克多巴胺测定结果的不确定度主要来源于重复测量;特布他林测定结果的不确定度主要来源于重复测量;沙丁胺醇测定结果的不确定度主要来源于标准物质的浓度。     

荧光分析法测定维生素C

维生素C经Cu2 氧化为脱氢抗坏血酸,与苯甲酸及十六烷基三甲基溴化铵产生荧光协同增敏作用。提出一种新的测定维生素C的高灵敏荧光分析法,建立了测定维生素C的适合条件。该方法的的线性范围为0.02~8.0μg/mL,检出限为0.006 5μg/mL。对3.0μg/mL的维生素C测定6次,测定结果的相对标准偏差为0.12%。将该法用于西红柿、果珍以及维生素C药片中维生素C含量的测定,加标回收率为96.7%~100.5%。     

涂丝型聚氯乙烯膜-硫酸沙丁胺醇电极的研制与应用

采用电位分析法测定猪肉中硫酸沙丁胺醇的含量。以硫酸沙丁胺醇与四苯硼钠形成的缔合物为电活性物质制备了涂丝型硫酸沙丁胺醇选择电极,并对其各项性能进行测定。结果表明:电极对硫酸沙丁胺醇有很好的能斯特响应。电极响应的范围为1.0×10-5~1.0×10-1 mol·L-1,级差电位为31mV·pc-1,测定下限(10S/N)为6.5×10-6 mol·L-1。用该电极对猪肉中硫酸沙丁胺醇的含量进行测定,测定结果与标准方法测定值相符。     

酶荧光毛细管分析法测定微量血清中乳酸脱氢酶活性

基于丙酮酸/还原型辅酶I/乳酸脱氢酶(LDH)/乳酸/氧化型辅酶I荧光猝灭体系和荧光毛细管分析技术,建立了可用于微量样品中LDH酶活性测定的方法。优化的测定条件为:激发及发射波长分别为350和460nm;测定温度为25℃;酸度为pH 6.5;NADH浓度为300μmol/L;丙酮酸浓度为1.2mmol/L。本方法的测定范围为50～1500IU/L,检出限为30IU/L,相对标准偏差2.1%～2.2%(n=10),回收率在96.4%～105%范围内。本方法操作简单,每次测定仅需样品2.0μL、试剂18.0μL,分析速度约为30样/h,利用本方法测定了微量血清中LDH的活性。     

碱熔-电感耦合等离子体发射光谱法测定锡矿石中锡

本文采用过氧化钠碱熔消解样品,电感耦合等离子体发射光谱( ICP-AES)法,对锡矿石中锡含量进行了测定。当样品称样量为0.2g时加入2g过氧化钠就能使样品消解完全。为避免水解对测定结果的影响,样品处理后应尽快进行测定。本方法测定锡的检出限为38.4mg/ kg,12次平行测定的相对标准偏差小于5%,对标准物质的测定结果也令人满意。     

三波长分光光度法测定葡萄籽中总黄酮含量

采用三波长分光光度法测定了葡萄籽中的总黄酮含量,方法有效地消除了吸收峰不对称及干扰组分对定量分析造成的影响。该法分别采用芦丁和原花青素两种物质为标准进行测定,以芦丁为标准测定的线性范围为0～10.8μg/mL,回收率为96.7%～110.0%,相对标准偏差小于3.8%;以原花青素为标准测定的线性范围为0～3.0μg/mL,方法的回收率为93.3%～104.0%,相对标准偏差小于2.4%。两种物质作为标准物质对测定结果无显著差异。     

原子吸收法测定添加剂和润滑油中钙、钡、锌含量

本方法适合测定添加剂和润滑油中的钙、钡、锌含量。样品处理使用灰化和硝酸溶解灰分法。测定钡时,使样品溶液在pH>10的条件下,加入0.25MEDTA和用氯化钾溶液稀释后进行原子吸收测定。钙和锌的测定采用空气/乙炔火焰,钡用氧化五氮/乙炔火焰测定,其方法的精密度按相对标准偏差计钙为3.3%、钡为4—8%、锌为9.3%。     

Determination of Penicillins in Milk by a Dual-Optrode Biosensor

Penicillins are the most frequently found antibiotic residues in milk, as they are commonly used for the treatment of bacterial infections in cows. In the present study, we introduce a method for the rapid detection of penicillin residues in raw milk based on the determination of glucose concentration in milk with a dual flow-through biosensor. The molar concentration of glucose in milk is typically over 500 times lower than the concentration of lactose and is highly dependent on the rate of lactose hydrolysis, which is catalyzed by β-galactosidase. Glucose concentrations in milk change with variation in the β-galactosidase activity. β-Galactosidase is an enzyme produced in the microbiota in milk and its activity is inhibited by benzylpenicillin. Spiking milk with benzylpenicillin lowers glucose concentrations in comparison to high-quality milk after short storage intervals. The presence of penicillin in the milk of treated animals resulted in decreased glucose concentrations in comparison with high-quality milk that contained no antibiotics. The glucose concentration in milk samples was followed by the system enabling the elimination of the effects of bacterial respiration in the output with reliable results in less than 1?min.     

醇类在芳烃溶剂中的缔合溶液热力学

用凝固点降低法测量了在C1-C4醇类的各异构物分别存在下, 苯和对二甲苯溶剂的活度系数γB。用Wiehe-Bagley(WB)模型对数据进行了处理, 得到各醇的自缔合常数KA及无限稀活度系数γA。在同一溶剂中, KA依下列顺序减小: 甲醇>乙醇>正丙醇>正丁醇; 正丙醇>异丙醇; 正丁醇>异丁醇>叔丁醇≥仲丁醇。各醇在对二甲苯中的KA均大于相应的在苯中的KA。     

Environmental aspects of tributyltin

The tributyltin species, the active ingredient in some antifouling paint formulations, is perhaps the most acutely toxic chemical to aquatic organisms ever deliberately introduced to water. It has been demonstrated to have an adverse effect on shellfish in France and England, and as a consequence the use of tributyltin-containing antifouling paints has been restricted in these countries. Other countries have banned the use of tributyltin-containing antifouling paints or are contemplating restrictions. This article reviews such environmental aspects of tributyltin as methods of analysis, toxicity, environmental occurrence, persistence and fate. Tributyltin concentrations in many locations may be high enough to cause chronic toxicity or harmful effects in some aquatic organisms, and in some locations the tributyltin concentrations may be high enough to be acutely toxic to some organisms. Biological degradation of tributyltin in water and sediment appears to be the most important factor limiting the persistence of tributyltin in aquatic environments. To some degree, then, the persistence of tributyltin in aquatic environments depends upon the nature of the ecosystem. Tributyltin exhibits low-to-medium persistence in water and moderate persistence in sediment. A summary is given of the regulatory status of tributyltin in some countries, and recommendations are made for further research.     

中国煤中铍的分布赋存特征研究

根据对中国不同矿区1018个煤层煤样和生产煤样铍含量数据的统计结果,分析了中国不同成煤时代、不同聚煤区煤中铍的分布特征。同时,根据对10个不同煤田煤样的实验室浮沉试验、煤岩分析等试验研究,运用Solari方法,计算了煤中各组分中铍的理论含量,讨论了中国煤中铍的赋存特征,尤其是铍在各种煤岩组分中的分布。研究表明,铍在煤中富集程度较高,但相对于世界煤中平均水平来说,中国煤中铍含量总体水平较低。煤中铍主要赋存于惰质组及伊利石粘土矿物中,在镜质组及其它矿物中含量较低。同时,中国大多数煤中铍的有机亲和性指数较高,不利于选煤过程中铍的脱除。     

Calibration methods for microdialysis sampling in vivo: muscle and adipose tissue

Calibration methods for microdialysis sampling were studied in the muscle and adipose tissue of rats. Both the delivery method and the no-net-flux method were used to determine the extraction efficiency (EE) of acetaminophen and caffeine in both tissues. There was no concentration dependence of the EE either in vitro or in vivo for either acetaminophen or caffeine. The EEs determined by the delivery and no-net-flux methods were not different. However, the EEs of both caffeine and acetaminophen determined in vitro were significantly higher than those determined in the muscle and adipose. This indicates that mass transfer in the tissue is the rate-determining factor for the EE in vivo. The relative difference between the EE in vitro and the EE in the muscle was smaller than the difference between the EE in vitro and the EE in the adipose. In addition, the EE in the muscle decreased more than the EE in the adipose after the animal was euthanized. This indicated that exchange between the extracellular fluid and plasma is the rate-determining step in mass transport relative to microdialysis sampling. This has a more significant effect on the EE in the muscle than the EE in the adipose. Both the delivery and no-net-flux methods can be used to calibrate microdialysis probes in the muscle and adipose.     

延边地区65～108岁健康老人头发中锌、铜、铁、锰、镁的含量

用原子吸收光谱法测定延边地区317名65～108岁老人头发中锌、铜、铁、锰、镁含量，观察不同民族、性别、年龄老人这些元素的差异。结果表明：1.朝鲜旗发锌低于汉族，满族发铜低于汉族、朝鲜族，汉族发镁高于朝鲜族、满族，发铁、发锰在汉、朝、满民族之间无区别。2．汉族、朝鲜族男发锌高于女性，汉族女性发铜高于男性，发铁、发锰、发镁在性别之间无区别。3、90岁组朝鲜族发锰、发镁低于65岁、76岁组，朝鲜族发锌、发铜、发铁在65～108岁之间无统计学意义。     

Analytical strategies to determine antibiotic residues in fish

The accelerated growth of aquaculture has resulted in a series of harmful effects to human health. The widespread and unrestricted use of antibiotics in this industry, to prevent bacterial infections, leads to remaining amounts in the aquatic environment. This has resulted in the emergence of antibiotic-resistant bacteria in aquaculture environments, in the increase in antibiotic resistance in fish pathogens as well as in the transfer of these resistance determinants to human pathogens. Moreover, the use of large amounts of antibiotics may lead to the presence of residual antibiotics in fish tissue and fish products. Fluoroquinolones, tetracyclines, penicillins, sulphonamides and other antibiotics, exhibiting activity against both Gram-positive and Gram-negative bacteria, are widely used for the treatment and prevention of diseases in fish. An extended and comprehensive review on the recent analytical methodologies concerning antibiotic residues in fish reported in the literature is provided in the present article. Emphasis is given on sample preparation regarding isolation and purification, chromatographic conditions and method validation according to legislation. Results of published assays are comparatively presented and criticised.     

Graves病患者经131I治疗后血浆和红细胞锌含量的变化及其临床意义

为研究Graves病(GD)患者经^131I治疗后血浆和红细胞锌(Zn)含量的变化及其临床意义，采用原子吸收分光光谱法(AAS)和放射免疫分析法(Rn)分别检测了40例GD患者、20例经^131I治疗后甲状腺功能恢复至正常水平GD患者与30名健康人血浆和红细胞Zn的含量以及血浆甲状腺激素水平。结果表明，GD组红细胞Zn含量明显低于对照组(P＜0．01)；血浆Zn含量虽略低于对照组，但无统计学意义(P＜0．05)；且Zn与FT4呈明显负相关(P＜0．01)、与TSH呈正相关(P＜0．05)。GD治疗缓解组红细胞Zn明显高于治疗前(P＜0．01)，血浆Zn明显低于治疗前(P＜0．05)；红细胞Zn检测GD的敏感性与特异性分别为95．0％与96．7％。提示GD患者存在红细胞Zn含量改变，甲状腺激素可能干扰红细胞Zn的代谢，同时测定红细胞Zn可作为GD的临床诊断、治疗以及疾病转归的参考指标。     

Shear-induced crystallization in phase-separated blends of isotactic polypropylene with ethylene-propylene-diene terpolymer

The compatibility between isotactic polypropylene(i PP) and ethylene-propylene-diene terpolymer(EPDM) in the blends was studied. SAXS analysis indicates that i PP and EPDM phases in the binary blend are incompatible. Isothermal crystallization behaviors of i PP in phase-separated i PP/EPDM were studied by in situ POM equipped with a Linkam shear hot stage. It was found that typical spherulites of i PP were formed both in neat i PP and in i PP/EPDM blends. The radial growth rate(d R/dt) of spherulites of i PP in the blend was not influenced by EPDM phases. Further investigations on isothermal crystallization of i PP in i PP/EPDM after shear with a fixed shear time showed that the crystallization rate of i PP in the blends increased with increasing shear rates, whereas, the crystallization rate was much lower than that of neat i PP. WAXD results showed that ?-crystal i PP was formed in neat i PP as well as in i PP/EPDM blends after shearing and the percentage of ?-crystal bore a relationship to the applied shear rate. The presence of EPDM resulted in lower percentage of ?-crystal in the blends than that in neat i PP under the same constant shear conditions. SAXS experiments revealed that shear flow could induce formation of oriented lamellae in i PP and i PP in the blends, and the presence of EPDM led to a reduced fraction of oriented lamellae.     

Versican undergoes specific alterations in the fine molecular structure and organization in human aneurysmal abdominal aortas

Versican is the major matrix proteoglycan in aortic wall and participates in various biological functions of the tissue. In the present study the molecular characteristics of versican isolated from normal human aorta as well as those of versican expressed in aneurysmal aortic tissue were examined. Versican was isolated by combined anion-exchange and gel permeation chromatography and was further characterized by high-performance liquid chromatography, polyacrylamide gel electrophoresis and immunoblotting. In both tissues versican is exclusively substituted with chondroitin sulfate chains, in contrast to other human tissues where both chondroitin and dermatan sulfate chains are attached onto versican core proteins. Except for the significant decrease in the concentration of versican in the aneurysmal tissue, this PG undergoes specific alterations in the aneurysmal tissue. The molecular size of versican isolated from diseased tissue is decreased with a simultaneous increase in the ratio of glycosaminoglycan to protein in this tissue. The latter reflect the extensive fragmentation of versican in the diseased tissue and most probably the generation of shorter peptides enriched to glycosaminoglycan chains. Although the size of chondroitin sulfate chains is identical in both versican preparations, a significant increase in the percentage of 6-sulfated disaccharides is observed in chondroitin sulfate chains of versican in aneurysmal aortas, which is accompanied by decrease in 4-sulfated and non-sulfated units.