Determination of phenylalanine isotope ratio enrichment by liquid chromatography/time- of-flight mass spectrometry

The application of time-of-flight mass spectrometry to isotope ratio measurements has been limited by the relatively low dynamic range of the time-to-digital converter detectors available on commercial LC/ToF-MS systems. Here we report the measurement of phenylalanine isotope ratio enrichment by using a new LC/ToF-MS system with wide dynamic range. Underivatized phenylalanine was injected onto a C18 column directly with 0.1% formic acid/acetonitrile as the mobile phase. The optimal instrument parameters for the time-of-flight mass spectrometer were determined by tuning the instrument with a phenylalanine standard. The accuracy of the isotope enrichment measurement was determined by the injection of standard solutions with known isotope ratios ranging from 0.02% to 9.2%. A plot of the results against the theoretical values gave a linear curve with R2 of 0.9999. The coefficient of variation for the isotope ratio measurement was below 2%. The method is simple, rapid, and accurate and presents an attractive alternative to traditional GC/MS applications.     

富勒烯及其衍生物的质谱研究

本文制备了一系列富勒烯及其衍生物，并利用多种质谱技术进行了鉴定、表征、揭示了它们在离子源条件下的稳定性及解规律。这些富勒烯及其省生物在ＦＤＭＳ、ＩＳＭＳ中均得到了较强的准分子离子峰且碎片峰很少。结果表昨ＦＤＭＳ，ＬＳＩＭＳ技术均适于富勒烯及其衍生物的定性分析，是目前富勒烯分析鉴定中较好的方法。     

2-取代亚肼基-1,3-二硫杂环戊烷类化合物的合成及其生物活性研究

以取代苯甲醛、取代吡啶和取代苯甲酸酯等为原料合成了 10种含硫杂环化合物 (其中 2a～ 2g化合物为国内外未见报道 ) .在合成过程中采用了超声波技术 ,极大地缩短了反应时间 ,提高了收率 .所得化合物的结构经IR ,1 HNMR ,MS和元素分析证实 .对其生物活性进行了初步测试 ,结果证明一些化合物具有良好的抑菌或杀菌作用 ,其中 2b ,2c ,2e ,2h ,2i和2j对大肠杆菌 ( 10 40 7号 )的抗菌效果与CET和SMZ相当 ;2b ,2c ,2f对草绿色链球菌 ( 112 3号 )的抗菌效果与CET和SMZ相当 .     

气相色谱-负化学源质谱联用法测定菊酯类农药

通过固相萃取-气相色谱-负化学离子源质谱技术建立了11种拟除虫菊酯类农药残留的检测方法，并应用于茶叶农残检测。样品经乙酸乙酯提取后，用串联的活性炭和中性氧化铝固相萃取柱选择性地富集茶叶中待测组分，再由气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定。方法简单快速，一次进样就能得到11种菊酯残留结果；准确度和精密度高，在0．016μg／kg、0．032μg／kg和0．064μg／kg3个添加水平下的回收率在70％～110％之间，CV≤7．4％；选择性好，消除了色素和其它杂质干扰；灵敏度高，检出限低，除了氯菊酯为10μg／kg外，其它菊酯检出限都在μg/∥kg级，七氟菊酯则达到了0．02μg／kg。     

聚丙烯酰胺双向凝胶电泳法分析变色人发角蛋白组成

报道了一种用双向聚丙烯酰胺凝胶电泳分析经Ｓ－羧甲基化修饰的变色人发角蛋白样品的方法，以含８ｍｏ１／Ｌ脲变性凝胶电泳做第一向，ＳＤＳ－ＰＡＧＥ做第二向。不同处理的变色人发得到有差别的双向电泳图谱，即不同处理方法得到的人发蛋白质组成有差异。以此可做为人发变色处理的一个定性方法。     

Design, synthesis and antifungal activity of novel triazole derivatives

Twenty-three 1 -(1H-1,2,4-triazole-1 -y1)-2-(2,4-difluorophenyl)-3-(iV-cycloproyl-N-substituted-amino)-2-propanols were designed and synthesized on the basis of the active site of lanosterol 14α-demethylase. In vitro antifungal activities showed that some of the title compounds had higher antifungal activity and broader antifungal spectrum than fluconazole.     

Preparation of Europium Induced Conformation—specific anti—calmodulin Monoclonal Antibody

Monoclonal antibody technique was employed to detect the conformational difference of CaM induced by metal ions. A trivalent europium ion induced conformation-specific anti-calmodulin monoclonal antibody was successfully prepared with europium-saturated calmodulin as antigen.     

药用缓释辅料——羟丙基甲基纤维素的合成及其缓释性能的研究

本文研究了药物缓释材料HPMC的合成方法,探讨了碱纤维素制备,醚化剂浓度,混合醚化剂配经以及产品后处理对高粘度HPMC的影响。本文还初步对KCl,氨茶碱,硝酸异山梨醇酯等药物采用合成的HPMC作辅料,进行了缓释制剂的研究,结果表明合成的HPMC具有满意的缓释性能。     

离子注入修饰电极检测硝基苯

离子注入是一种新技术，可按人们的意愿和需要，将不同的离子注入不同的基本电极表面，制成具有催化活性强，稳定性高，重现性好等特点的修饰电极。作者研究了离子注入钴和注入镍的玻碳电极在０．１ｍｏｌ／ＬＨＡｃ－ＮａＡｃ缓冲溶液中硝基苯的行为及测定。