柱后紫外衍生-离子色谱法测定天然矿泉水中硼酸

目的 建立天然矿泉水中硼酸的柱后衍生-离子色谱测定法.方法 样品中的硼酸通过离子色谱柱分离,柱后紫外衍生法测定.结果 硼酸在0.3～ 10.0 mg/L范围内线性关系良好,相关系数为0.999 6;以3倍信噪比计算,本法的检出限为0.3 mg/L;方法相对标准偏差为1.8％～2.2％,回收率为94.0％～98.7％.结论 该方法线性好,灵敏度高,专属性强,可应用于天然矿泉水中硼酸含量的检测.     

A unified software framework for deriving,visualizing, and exploring abstraction networks for ontologies

Software tools play a critical role in the development and maintenance of biomedical ontologies. One important task that is difficult without software tools is ontology quality assurance. In previous work, we have introduced different kinds of abstraction networks to provide a theoretical foundation for ontology quality assurance tools. Abstraction networks summarize the structure and content of ontologies. One kind of abstraction network that we have used repeatedly to support ontology quality assurance is the partial-area taxonomy. It summarizes structurally and semantically similar concepts within an ontology. However, the use of partial-area taxonomies was ad hoc and not generalizable. In this paper, we describe the Ontology Abstraction Framework (OAF), a unified framework and software system for deriving, visualizing, and exploring partial-area taxonomy abstraction networks. The OAF includes support for various ontology representations (e.g., OWL and SNOMED CT’s relational format). A Protégé plugin for deriving “live partial-area taxonomies” is demonstrated.     

柱前衍生化HPLC-UV法测定天麻胶囊中齐墩果酸的含量

目的建立天麻胶囊中齐墩果酸的含量测定方法。方法以对硝基苯甲酰氯为衍生化试剂对齐墩果酸进行柱前衍生,用HPLC-UV法对衍生物进行测定,色谱条件为:Diamonsil(钻石)C18色谱柱(200 mm×4.6 mm,5μm),乙腈-0.2%磷酸水溶液(95∶5)为流动相,流速1.0 ml/min,检测波长254 nm。结果成功建立了天麻胶囊中齐墩果酸的柱前衍生测定法,衍生物线性回归方程为:Y=90 374X+90.208(r=0.999),在0.39-6.20μg范围内线性关系良好。结论柱前衍生化HPLC-UV法可用于天麻胶囊中齐墩果酸的含量测定,衍生物为对硝基苯甲酸齐墩果酸酯,检测波长红移至254 nm,方法准确,灵敏度高,可为天麻胶囊的质量评价提供依据。     

柱前衍生HPLC测定阿胶中17种水解氨基酸含量

目的 建立柱前衍生高效液相色谱法(HPLC)同时测定阿胶中17种水解氨基酸含量的方法.方法 用6 mol/L盐酸溶液水解阿胶中的氨基酸,以异硫氰酸苯酯为柱前衍生试剂;用Hypersil BDS C18柱(200 mm×4.6 mm,5μm),梯度洗脱,流速为1.0 mL/min,检测波长为254nm,柱温为30℃.结果 17种氨基酸在60 min内均可得到很好的分离,回收率为97.4％～1 00.1％,RSD为1.6％～3.4％.结论 建立的方法可靠,可用于阿胶中17种水解氨基酸的含量测定.     

柱前衍生化–高效液相色谱法测定蒙古黄芪多糖中单糖的组成

目的 测定蒙古黄芪多糖中的单糖组成。方法 蒙古黄芪多糖样品用三氟乙酸溶液水解成单糖,用1-苯基-3-甲基- 5-吡唑啉酮（PMP）衍生化,采用HPLC法于245 nm波长处检测各单糖。结果 蒙古黄芪多糖由甘露糖、鼠李糖、半乳糖醛酸、葡萄糖、阿拉伯糖组成,物质的量比分别为0.02∶0.05∶0.17∶1∶0.18。结论 此方法简单、快速、重复性好,可用于蒙古黄芪多糖中单糖组成分析。     

柱前衍生化HPLC法测定黄河滩枣多糖的单糖组成

目的建立PMP(1-苯基-3-甲基-5-吡唑啉酮)柱前衍生化HPLC法测定黄河滩枣多糖的单糖组成。方法采用水提醇沉法提取黄河滩枣多糖,多糖水解后进行PMP衍生化,HPLC法测定黄河滩枣多糖的单糖组成及摩尔比,并对等度和梯度洗脱两种模式的测定结果进行分析比较。结果黄河滩枣多糖由D-甘露糖、L-鼠李糖、D-半乳糖醛酸、D-葡萄糖、D-半乳糖、L-阿拉伯糖等六种单糖组成,它们的摩尔比约为0.54∶0.50∶0.27∶2.03∶5.40∶1.00,等度和梯度洗脱测定结果基本一致。结论本实验改进的等度洗脱方式更加简便易行,快速准确,适用于黄河滩枣多糖的单糖组成分析。     

FMOC-Cl柱前衍生化HPLC法测定注射用帕米膦酸二钠的含量

目的:建立氯甲酸-9-芴甲酯(FMOC-Cl)柱前衍生化HPLC法测定注射用帕米膦酸二钠的含量。方法:碱性条件下供试品与FMOC-Cl进行衍生化反应,采用Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-0.4%EDTA溶液(用1 mol·L-1氢氧化钠溶液调节pH至7.2)(25∶75),流速1 mL·min-1,检测波长为265 nm。结果:帕米膦酸二钠浓度在0.05～1.00 mg·mL-1范围内与峰面积呈良好关系(r=0.9998),平均回收率为101.0%(n=9)。结论:该方法专属性好,适合用于注射用帕米膦酸二钠的含量测定。     

柱前手性衍生化-HPLC法测定人血浆和尿液中D-谷氨酸和D-丝氨酸的浓度

目的:建立手性分离D-谷氨酸和D-丝氨酸的方法,测定人血浆和尿液中D-谷氨酸和D-丝氨酸的浓度。方法:12对极性氨基酸标准液混合后,加入衍生化试剂邻苯二甲醛、N-乙酰-L-半胱氨酸衍生化后,采用高效液相色谱法进样测定。色谱柱为大连依利特HypersilC18,流动相为甲醇-50mmol·L-1醋酸铵缓冲液(pH6.0),梯度洗脱,流速为1.0mL·min-1,柱温为室温,进样量为20μL,荧光检测波长为350nm(激发波长)、450nm(发射波长)。结果:D-谷氨酸、D-丝氨酸检测浓度分别在0.5～20、0.5～80nmol·L-1范围内线性关系良好,平均方法回收率分别为96.4%～103.6%、97.1%～100.5%,日内、日间RSD均<8%。测得正常人血浆中D-谷氨酸和D-丝氨酸平均含量分别为(2.43±0.37)、(1.07±0.11)nmol·mL-1,尿样中未能检测到2种D型氨基酸。结论:本研究建立的手性分离测定D-谷氨酸和D-丝氨酸的分析方法可行,可用于测定人血浆和尿液中二者的浓度。     

The influence of time preparation on motor processes assessed by surface Laplacian estimation

OBJECTIVE: The present study was aimed at testing whether foreperiod duration affects the activity recorded over the primary sensorimotor cortices during the reaction time. METHODS: The foreperiod duration (500 or 2500 ms) was varied across blocks of trials during a between-hand choice reaction time task; surface Laplacians were estimated from EEG recordings by the source derivation method. RESULTS: Reaction time was shorter for the 500 ms foreperiod than for the 2500 ms foreperiod. A contralateral negativity/ipsilateral positivity pattern showed up over the primary sensorimotor cortices. The time between the contralateral negativity onset and the electromyographic onset was shorter for the 500 ms foreperiod than for the 2500 ms foreperiod, which suggests that the foreperiod affects the implementation of the motor command. Furthermore, the interval between the onset of the voluntary electromyographic activity and the mechanical response was shorter for the 500 ms foreperiod than for the 2500 ms foreperiod. CONCLUSIONS: These results indicate that time preparation affects both central and peripheral motor processes.     

气-质联用结合衍生化法分析血浆中甲基苯丙胺和氯胺酮

目的:考察家兔血浆中甲基苯丙胺和氯胺酮同时衍生化后GC/MS检测分析结果。方法:血浆样品中加入内标物丙基解痉素(SKF525A)后碱化,乙醚萃取,三氟醋酸酐(TFA)衍生化,GC/MS全扫描定性、内标法和工作曲线法定量分析。结果:甲基苯丙胺和氯胺酮在血浆中的线性检测范围分别为0.010 0~10.0μg.mL·1和0.010 0~20.0μg.mL·1;方法回收率为95.26%~101.10%;日内及日间相对标准差均小于15%。结论:建立了衍生化后同时测定血浆中甲基苯丙胺及氯胺酮的GC/MS定性定量分析方法,该法简便、灵敏、重复性好,适用于甲基苯丙胺和氯胺酮混合滥用中毒案例的快速鉴定。