薄膜定量分析中的Auger线型分析方法

采用Ａｕｇｅｒ线型分析方法－因子分析方法和已知组元强度的定量解谱技术，对电子束辅助Ｎ离子注入Ｓｉ和磁控溅射方法制备的ＴｉＮｘ薄膜的高分辨率俄歇电子能谱（ＡＥＳ），进行了定量分析。讨论了化学成分对ＡＥＳ线型的影响及线型分析技术的有效性和应用范围。     

Metabonomic analysis of hepatitis B virus-induced liver failure： identification of potential diagnostic biomarkers by fuzzy support vector machine

Hepatitis B virus （HBV）-induced liver failure is an emergent liver disease leading to high mortality. The severity of liver failure may be reflected by the profile of some metabolites. This study assessed the potential of using metabolites as biomarkers for liver failure by identifying metabolites with good discriminative performance for its phenotype. The serum samples from 24 HBV-indueed liver failure patients and 23 healthy volunteers were collected and analyzed by gas chromatography-mass spectrometry （GC-MS） to generate metabolite profiles. The 24 patients were further grouped into two classes according to the severity of liver failure. Twenty-five eommensal peaks in all metabolite profiles were extracted, and the relative area values of these peaks were used as features for each sample. Three algorithms, F-test, k-nearest neighbor （KNN） and fuzzy support vector machine （FSVM） combined with exhaustive search （ES）, were employed to identify a subset of metabolites （biomarkers） that best predict liver failure. Based on the achieved experimental dataset, 93.62% predictive accuracy by 6 features was selected with FSVM-ES and three key metabolites, glyeerie acid, cis-aeonitie acid and citric acid, are identified as potential diagnostic biomarkers.     

Determination of risperidone in human plasma by HPLC-MS/MS and its application to a pharmacokinetic study in Chinese volunteers

This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry （LC-MS/MS） assay for determination of risperidone （RIS） in human serum using paroxetine as an internal standard （IS）. An Alltima-C18 column （2.1 mm×100 mm, 3 μm） and a mobile phase consisting of 0.1% formic acid-acetonitrile （40：60, v/v） were used for separation. The analysis was performed by selected reaction monitoring （SRM） method, and the peak area of the m/z 411.3→191.1 transition for RIS was measured versus that of the m/z 330.1→192.1 transition for IS to generate the standard curves. The assay linearity of RIS was confirmed over the range 0.25-50.00 ng/ml and the limit of quantitation was 0.05 ng/ml. The linear range corresponds well with the serum concentrations of the analytes obtained in clinical pharmacokinetic studies. Intraday and interday relative standard deviations were 1.85%-9.09% and 1.56%-4.38%, respectively. The recovery of RIS from serum was in the range of 70.20%-84.50%. The method was successfully applied to investigate the bioequivalence between two kinds of tablets （test versus reference products） in 18 healthy male Chinese volunteers. The result suggests that two formulations are bioequivalent.     

火焰原子吸收法测定粮食中锌

本文采用火焰原子吸收法直接测定粮食中的锌含量 .方法简单、快速、准确 .结果令人满意     

二阶导数光谱法测定蛋白质的含量

导数光谱是紫外可见分光光度法中用以排除干扰的一种技术。本文用日立220—A紫外可见分光光度计中测定了血清蛋白质的含量。通过实验得出的线性回归方程为D=155.24c—0.346;相关系数r=0.9998,样本平均回收率为100.05％,精度试验d=0.077,S=0.418,dx=0.027,Sx=0.148。此法重现好,变异系数(CV)<±1％,此法简单,快速,可用于血清蛋白质的测定。     

山苍子油毛细管气相色谱分离及成分的色/质谱鉴定

首次采用毛细管色谱及色/质联用技术对云南山苍子油进行分离及成分直接定性,并提出了对其主成分柠檬醛的一种恒温毛细管色谱定量方法。     

卟啉类光敏剂的制备及其研究(Ⅴ)──血卟啉及其衍生物的激光荧光光谱及单态氧的测定

卟啉、氧和光是光化治癌的三个基本要素。本文测定了血卟啉及其衍生物的荧光 光谱及单态氧的相对量子产额。结果表明，血卟啉的荧光强度和单态氧的量子产 额较高，它们均为有效的光敏剂。     

火焰原子吸收法测定血清中的痕量铬

采用0.2％柠檬酸钠和0.2％硫酸钠水溶液作为原子吸收法测定血清中痕量够的介质,能有效抑制共存元素的干扰,并使铬的吸光度有较大的增值。它能克服通常所采用的有机溶剂萃取预处理手段的明显缺点,而且简便快速。本法灵敏度为0.056ug/ml/1％。检出限为0.007ug/ml,变异系数为2.7％。     

离子色谱-质谱联用法测定4-甲基咪唑的含量

为了简单、方便地精确定量和定性样品中的4-甲基咪唑,建立了一种采用阳离子交换色谱-质谱联用(IC-MS)技术准确检测4-甲基咪唑含量的新方法,该方法的检出限为0.25μg/L,线性范围为2.5~200μg/L,线性相关系数为0.999 7,相对标准偏差为2.32%~4.25%,加标回收率为92.7%~96.3%.使用该方法对焦糖色素、可乐等样品进行检测,结果表明,该方法具有分离度高、灵敏度高、定量准确、精密度高、检出限低的特点.     

固相萃取GC-MS法测定蜂蜜中挥发性成分

通过比较溶剂萃取(SE)、同时蒸馏萃取(SDE)和固相萃取(SPE)3种样品前处理方法,确定蜂蜜中挥发性成分的最优提取方法,建立蜂蜜中挥发性成分的固相萃取-气相色谱-质谱(GC-MS)检测方法.以亲水性HLB固相萃取柱为对象,考察并优化HLB柱的淋洗与洗脱条件,确定HLB柱在以1mL的V(甲醇)∶V(水)=1为淋洗剂,1mL二氯甲烷为洗脱剂的条件下对蜂蜜中挥发性成分提取效果最好,GC-MS可分析出蜂蜜中47种挥发性成分.