N-乙基-N-苄基间磺酸苯胺中异构体的分离研究

对N-乙基-N-苄基间磺酸苯胺中间位、对位及邻位异构体进行了分离研究，用苯甲醛邻磺酸与N-乙基-N-苄基闯磺酸苯胺混合物缩合，制成衍生物，再用HPLC(色谱柱：CLC-ODS，检测波长：254nm，流动相：甲醇／四丁基溴化铵=60％／40％)分离，可使异构体得到有效分离，并能判断N-乙基-N-苄基间磺酸苯胺商品中间位物主含量的高低。     

Kinetics of the enzymatic degradation of poly(vinyl acetate) in solution

The enzymatic degradability of poly(vinyl acetate) was investigated in toluene solutions at various temperatures with hog pancreas lipase. The polymer degraded by specific scission to yield oligomeric products with a molecular weight of 700. Continuous distribution kinetics were used to determine the rate coefficients. The variation of the rate coefficients with the temperature indicated an optimum at 55°C. The p‐toluene sulfonic acid catalyzed degradation of poly(vinyl acetate) was also investigated. The degradation mechanism was random chain scission, and the energy of activation for degradation was determined from the variation of the rate coefficients with the temperature. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 2579–2582, 2003     

黄芩苷标样制备及其固相萃取-HPLC测定研究

采用超声波振荡-醇提取酸沉淀法代替传统的水提酸沉淀法从黄芩中提取黄芩苷粗品,再经分步精制得其纯品,同时提出了固相萃取-高效液相色谱法测定黄芩饮片以及几种中药制中黄芩苷含量的新方法;根据待测样品的差异,选择不同的前处理手段,采用W aters P lus-C18小柱固相萃取预分离,以CH3OH-H2O-HAc为流动相,测试样品中的黄芩苷得以分离和测定。新方法标准回收率92%~103%,RSD为1.4%~12.2%。     

三唑磷·毒死蜱乳油的液相色谱分析

以ODS色谱柱,UV246 nm为检测波长,用甲醇:水=90∶10(V/V)作为流动相,在ODS色谱柱上同柱液相色谱法测定三唑磷、毒死蜱的含量。方法的变异系数三唑磷为0.41%,毒死蜱为0.35%,三唑磷的回收率为98.9~100.7%,毒死蜱回收率为99.5%~100.6%。相关系数三唑磷为0.9968,毒死蜱为0.9999。     

Characterization of the TAG of peanut oil by electrospray LC-MS-MS

A study of processed peanut oil was undertaken to assess the utility of HPLC combined with tandem MS to obtain data easily regarding the number of TAG of fats and oils and their FA composition. Mass chromatograms and spectra corresponding to only TAG of a single M.W. were obtained for the full range of TAG in the sample. Analysis of the mass spectra allowed the identification of more than 160 TAG in the sample by their FA composition. In addition, it was possible to estimate relative abundances of the TAG and suggest the position of the FA on glycerol for a limited number of cases. This technique greatly simplifies the task of assigning FA to coeluting TAG and facilitates identification of TAG present in trace quantities in mixtures, with possible application in circumstances where such trace TAG could be significant markers. Results are quickly obtained without extensive sample preparation or prefractionation of the sample.     

HPLC法研究C.I.Reactive Red 24水解反应动力学

采用反相离子对高效液相色谱法(HPLC)研究了C.I.Reactive Red 24 水解反应动力学.当染料溶液中羟基过量时, 可视为一级反应; -d[A]/dt=k[A].在pH=13时, ln(A0/A)与反应时间t呈线性关系; 95℃时的水解反应速率常数K(0.0599)比70℃时的k(0.0101)高约4倍; pH为13时, 反应速率常数K(5.99×10-2)比8.5时的k(4.8×10-3)高约11.5倍; pH值每升高1, 染料的水解速率相应提高1.5倍.     

高效液相色谱法测定虫草黄酒中虫草素的研究

采用高效液相色谱法建立了虫草黄酒中虫草素含量的测定方法,探讨了虫草素提取条件,分析了流动相组成、柱温、波长对检测结果的影响.研究表明：色谱柱为Waters Symmetry C18柱,流动相为甲醇∶水=15∶85,流速为1mL/min;检测波长为288nm,柱温为40℃时分离、检测效果最好;方法检出限为0.05ng.该测定方法在黄酒质量控制方面具有应用价值.     

高效液相色谱法测定菊蓝抗流感片中蒙花苷含量

建立菊蓝抗流感片中蒙花苷的含量测定方法。采用高效液相色谱法,DiamonsilTMC18柱(250m×4.6m,5μm),流动相为甲醇-水-冰醋酸(43∶57∶1),检测波长为326nm。蒙花苷在0.251 2～2.512μg的范围内具有良好的线性关系,r=0.999 8;平均回收率为98.9%(RSD为0.3%)。可为菊蓝抗流感片的质量控制提供依据。     

钆内嵌金属富勒烯的制备、分离及质谱表征

利用自制的电弧炉,通过电弧放电法合成了内嵌金属富勒烯Gd@C82,研究并获得了制备钆金属富勒烯的最佳工艺条件：摩尔比Gd：C=1：15,电流I=90～100A,氦气压力0．08MPa;探讨并获得了Gd@C82新的萃取分离条件：常温下以DMF为溶剂,抽真空至压强为0．01MPa下萃取;讨论了内嵌金属富勒烯的生成和分离机理。     

HPLC测定参芪片中人参皂苷Re的含量

建立了测定参芪片中人参皂苷Re含量的HPLC法.采用色谱柱为AT-330C18;流速为1.0mL/min;流动相为乙腈-0.05%磷酸溶液(2080);检测波长为203nm.人参皂苷Re得到了较好的分离,在0.3486～3.486μg范围内呈良好的线性关系.本法简便快捷,结果可靠,可用于参芪片中人参皂苷Re的含量测定.