ICP-AES法测定霍加拉特剂中7种金属元素

采用王水湿式消化处理样品,建立了ICP-AES法同时测定霍加拉特剂中Mn、Cu、Na、Al、Ca、Mg和Fe等7种金属元素的方法。通过谱线选择、条件优化和基体匹配等方法消除元素间干扰和基体效应,探讨了酸类型及酸度值对谱线强度的影响,研究了溶液浓度对精密度及线性相关系数的影响。方法的线性相关系数均大于0.999,Mn、Cu、Na、Al、Ca、Mg和Fe的最佳谱线分别为Mn257.610nm、Cu327.393nm、Na589.592nm、Al396.153nm、Ca317.933nm、Mg285.213nm、Fe238.204nm,相应的检出限分别为0.0008、0.0009、0.012、0.028、0.010、0.001、0.004μg/mL,对应测定值的相对标准偏差分别为0.34%、0.87%、0.87%、0.54%、0.48%、0.84%、0.55%,加标回收率为94.2%～104.4%。该方法简便、快捷、准确,可在测定其他催化剂中金属含量时推广应用。     

Analysis and determination of diterpenoids in unprocessed and processed Euphorbia lathyris seeds by HPLC-ESI-MS

Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV and mass, quantifying three diterpenoids L1, L2, and L8 in crude extracts of unprocessed and processed E. lathyris seeds by liquid chromatography/ electrospray ionization mass spectrometry （LC-ESI-MS）. The analysis was achieved on an Agilent Eclipse XDB-C18 column （4.6 mm× 150mm i.d., 5 μm） with an isocratic elution with a mobile phase consisting of water and acetonitrile at a flow rate of 0.25 mL/min at column temperature of 30 ℃ and UV detection was set at 272 nm. An ESI source was used with a positive ionization mode. The calibration curve was linear in the ranges of 9.9-79 μg/mL for Euphorbia factor Lb 3.8-30.5μg/mL for Euphorbia factor L2, and 1.0-20.6 μg/mL for Euphorbia factor LB. The average recoveries （n=6） of three diterpenoids were 98.39%, 91.10% and 96.94%, respectively, with RSD of 2.5%, 2.4% and 2.1%, respectively. The contents of the three diterpenoids in processed E. lathyris seeds were 3.435, 1.367 and 0.286 mg/g, respectively, which decreased more sharply than those in unprocessed E. lathyris seeds which were 4.915, 1.944 and 0.425 mg/g, respectively. The method is simple, accurate, reliable and reproducible, and it can be applied to control the quality of unprocessed and processed E. lathyris seeds.     

Chemiluminescence enzyme immunoassay based on magnetic nanoparticles for detection of hepatoceUular carcinoma marker glypican-3

Glypican-3 （GPC3） is reported as a great promising tumor marker for hepatocellular carcinoma （HCC） diagnosis. Highly sensitive and accurate analysis of serum GPC3 （sGPC3）, in combination with or instead of traditional HCC marker alpha-fetoprotein （AFP）, is essential for early diagnosis of I-ICC. Biomaterial-functionalized magnetic particles have been utilized as solid supports with good biological compatibility for sensitive immunoassay. Here, the magnetic nanoparticles （MnPs） and magnetic microparticles （MmPs） with carboxyl groups were further modified with streptavidin, and applied for the development of chemiluminescence enzyme immunoassay （CLEIA）. After comparing between MnPs- and MmPs-based CLEIA, MnPs-based CLEIA was proved to be a better method with less assay time, greater sensitivity, better linearity and longer chemiluminescence platform. MnPs-based CLEIA was applied for detection of sGPC3 in normal liver, hepatocirrhosis, secondary liver cancer and HCC serum samples. The results indicated that sGPC3 was effective in diagnosis of HCC with high performance.     

中国沿海（散货）运输市场月评（2011年11月）

11月份,国内沿海散货运输市场行情大幅下滑。11月30日,上海航运交易所（简称航交所）发布的沿海（散货）运价指数报收于1154．35点,较上月同期下跌7．4％,破年内新低。煤炭、金属矿石和粮食运价指数有不同程度下跌,原油和成品油运价指数保持平稳。     

氢氟醚电解液在锂金属电池中的应用研究

无负极锂金属电池存在容量损失快和循环寿命短的缺点。本文设计制备一种氢氟醚电解液,探究其在无负极锂金属电池中的应用。采用X射线衍射仪(XRD)和扫描电子显微镜(SEM)进行分析,结果表明该氢氟醚电解液对高面容量银碳基无负极锂金属电池的循环性能有着优良的改善作用。氢氟醚电解液减少了锂枝晶的产生,提高了沉积锂的致密性,在大于3 mAh/cm2的高面容量下,银碳基无负极锂金属电池在0.5C的倍率下50次循环后仍保持96.2%的平均库伦效率,展现了优良的循环性能和良好的倍率性能,1C倍率下容量保持率≥85%。     

海水中锌腐蚀产物的研究

着重研究了实验室模拟海水和天然海水中锌腐蚀产物的电化学特性。采用阴极极化法研究腐蚀产物的特性，以循环极化曲线评估腐蚀产物中锌化合物的种类和数量。结果表明，腐蚀产物主要由碱性羟基氯化物组成，而该物质能提高腐蚀产物层的致密度。从循环极化曲线中回滞圈的面积Q可求出试样表面被腐蚀产物包覆的面积，且发现在实验室和现场海水试验中，该值都随锌暴露时间的增长而增大。结果表明，腐蚀产物致密因子C=Q／Icorr对表征腐蚀产物附着层对氧扩散的屏蔽作用有重要意义。     

暴露在海水管路中X52钢的局部生物腐蚀

通过采用生物探针在海水管路内表面放置微生物，对X52管材进行为期60天的暴露试验以对微生物所引起的腐蚀进行研究。遭受严重腐蚀的表面上有不同大小和深度的点蚀，当除掉沉积在生物试样表面的生物膜后，能观察到大量的金属损失，这在管路正常使用的情况下是没有预料到的。通过测量各坑的深度，得到一条深度分布曲线。从X52钢的生物试样表面取下的生物膜用于人工培养不同的嗜氧菌或兼性菌，发现厌氧菌呈现负增长。根据16S rRNA基因序列的相似性，确定了嗜氧菌和兼性菌的形态和化学特性，结果显示这些嗜氧菌和兼性菌可能是这种环境下产生的一个新物种。     

半金属摩擦材料与灰铸铁滑动摩擦的磨屑成分分析

采用X射线衍射仪和能谱分析系统，对3种金属纤维增强半金属摩擦材料与灰铸铁在不同温度时发生滑动摩擦后的磨屑成分进行了分析，并结合扫描电子显微镜(SEM)观察到的摩擦材料表面形貌，分析了材料的磨损特性和机理。分析结果表明，含钢纤维材料Fe原子浓度达50％～60％，Cu、Ba、Ca、Al等元素的原子浓度在6％～10％；含黄铜纤维与紫铜纤维的材料副磨屑中，二者Fe原子浓度均较高，但其它元素的原子浓度为紫铜低于黄铜；紫铜材料体系的结合程度比黄铜好，填料不易脱落，但对对偶损伤稍大。