Simultaneous determination of six preservatives in facial mask by high performance liquid chromatography

建立了同时测定单片式面膜中苯甲酸、山梨酸、脱氢乙酸、苯氧乙醇、氯苯甘醚和碘丙炔醇丁基氨甲酸酯6种防腐剂的高效液相色谱方法.面膜经50%(体积分数)甲醇提取,采用C18色谱柱,以甲醇和乙酸铵溶液(0.02 mol·L~(- 1))为流动相进行梯度洗脱,流速为1.0 m L·min~(- 1),柱温30℃,苯甲酸、山梨酸、氯苯甘醚、苯氧乙醇和碘丙炔醇丁基氨甲酸酯的检测波长为235 nm,脱氢乙酸的检测波长为295 nm.6种防腐剂浓度在0.5~20μg·m L~(- 1)范围内与峰面积均呈现良好的线性关系,方法的加标回收率为88.1%~105.3%,相对标准偏差为1.7%~2.8%.方法操作简便、快速,重复性好,灵敏度高,可用于面膜中6种防腐剂的测定.The high performance liquid chromatographic method was developed for the simultaneous determination of six preservatives( benzoic acid,sorbic acid,dehydro acetic,phenoxyethano,chlorphenesin,iodopropynyl butylcarbamate) in facial mask. The samples were extracted with 50%( volume fraction) methanol,and then separated on a C18 chromatographic column by gradient elution at a flow rate of 1. 0 m L · min~(- 1)with methanol- ammonium acetate solution as the mobile phase. The column temperature was 30 ℃. The wavelength of detection for benzoic acid,sorbic acid,phenoxyethano,chlorphenesin,iodopropynyl butylcarbamate was 235 nm,but for dehydroacetic acid was295 nm. In the range of 0. 5 to 20 μg·m L~(- 1)the peak area of six preservatives showed a good linear relationship,the recoveries were 88. 1% to 105. 3% with the relative standard deviations 1. 7% to2. 8%. The method is simple,rapid,accurate and sensitive,which can be used for determination of six preservatives in facial mask.福建省科技重大专项专题资助项目(2011YZ0001-1);; 福建省教育厅科技项目(JA13451

Establishment of Single Tube Quantitative Detection Technology for Escherichia coli Assay Based on Fluorescent Method

通过研究培养温度、培养基pH值对大肠杆菌生长和培养液荧光强度的影响,确定44℃,培养液pH值7.0～7.5为大肠杆菌MUG酶荧光检测的最佳条件。通过研究培养时间和接种菌浓度与培养液荧光强度的关系,建立起基于荧光方法检测大肠杆菌的单管定量检测技术。通过与平板菌落计数法和最大可能数法比较发现单管定量检测法的相对标准偏差小于这两种常用的方法,而且更为快速、经济,适合用于大肠杆菌的定量检测。Influence of incubation temperatures and pH values of culture liquid on growth of Escherichia coli and the fluorescent intensity of culture liquid had been investigated.E.coli incubated at 44℃ in the culture liquid with a pH value in the range of 7.0～7.5 was found to be the best condition for fluorescent assay.Single tube technology to detect E.coli was established through the studies on the relationship between incubation time,inoculation quantity of E.coli and the fluorescent intensity of culture liquid.Relatively standard diversity of single tube detection technology was lower than those of colony-counting method and the most probably number method.The results indicated that the single tube quantitative detection method was fit for E.coli quantitative detection because of the several advantages such as less time-consuming and more economical compared with traditional methods.国家高技术研究发展计划项目(863计划项目)(No2002AA639600);; 福建省自然科学基金(NoB0410022

中药现代化基础理论研究的几点思考

我国中药现代化基础理论研究应立足于提高我国人口素质及健康水平，促进国民经济发展（国家目标）。以传统中医药理论为基础，以现代生物医学与技术为指导（指导思想），围绕以下几个方面来进行：（1）治疗常见病、疑难病、多发病新药的创制；（2）为创制新药所需要的稳..

Determination of Chemical Oxygen Demand in Seawater Based on the Technique of Aqueous-Phase Ozone Oxidation

基于溶解臭氧在水体中能够氧化鲁米诺产生发光现象,建立了一种利用流动注射液相化学发光技术(FI-CL)测定化学耗氧量(COD)的新方法。COD测定范围在0.6～24mg/L之间,适合海水监测。对实际海水水样的测定结果与碱性高锰酸钾法具有一致趋势,测定的相对标准偏差小于10%。Based on the chemiluminscence(CL)phenomena of ozonation luminol,a new method utilizing flowinjection chemiluminescence(FI-CL)was developed.The concentration range for chemical oxygen deˉmand(COD)determination ranged from0.6to24mg/L,which is suitable for COD determination in seawaˉter.Real marine samples were analyzed and the results showed that the results measured by the FI-CL method were consistent with those by the Mn method.The relative standard deviation for three repeated meaˉsurements of COD was less than10%by FI-CL.国家863计划海洋领域资助项目(2001AA635120

A COMPUTER PROGRAM of DATA A CQUISITION FOR MULTICHANNEL INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETER

介绍了用于多道电感耦合等离子体原子发射光谱仪数据采集程序，给出了程序的基本框架。该程序用MICrOSOfTVISuAlbASIC50编写，界面友好，操作方便，并可根据需要进行功能扩充。A computer program of data acquisition is developed for multichannel inductively couple plasma atomic emission spectrometer.The core of the program presented in this paper is written in Microsoft Visual Basic 5 0, which is easy to use and easy to extend.国家自然科学基

Separation and Identification of Metallothionein Isoforms and Sub-isoforms by Liquid Chromatography

建立了金属硫蛋白(MT)异构体及亚型异构体的色谱分离与质谱鉴别方法。将金属硫蛋白混合物通过弱阴离子DEAESephadexA 25离子交换柱,结合离线电感耦合等离子体质谱(ICP MS)对锌诱导金属硫蛋白的两个异构体MT 1和MT 2进行分离和检测;利用SephadexG 25凝胶排阻色谱柱对得到的两个金属硫蛋白异构体进行脱盐;探索脱盐后的金属硫蛋白异构体在不同色谱条件下的C18反相色谱柱上的保留行为,进而实现各个亚型异构体的分离;通过在线电喷雾质谱检测实现了对金属硫蛋白各个亚型异构体的鉴别。结果表明,通过优化色谱条件,由离子交换色谱及凝胶排阻色谱得到的金属硫蛋白各亚型异构体在酸性条件下均得到了良好的分离,质谱检测结果与前人的文献报道结果一致。该方法可使金属硫蛋白各异构体均达到最佳的分离效果。A method has been established for the separation and identification of metallothionein (MT) isoforms and sub-isoforms by liquid chromatography. A mixture of rabbit liver MT was separated on a DEAE A-25 weak anion-exchange chromatographic (AEC) column. Inductively coupled plasma-mass spectrometer (ICP-MS) was used for off-line detection of Zn in each fraction. The two main MT isoforms, MT-1 and MT-2, were isolated. The collected MT isoform fractions were then desalted by a homemade Sephadex G-25 size exclusion chromatographic (SEC) column. Afterwards, the sample was separated on a C_(18) reversed-phase column with UV detection at 210 nm. Different separation conditions were discussed and several sub-isoforms of MT were well separated at pH 2.0. The sub-isoforms were finally characterized by on-line HPLC-ESI-MS. The isoforms and sub-isoforms were well separated on a reversed-phase column under optimized chromatographic conditions and the detection results of ESI-MS were in agreement with the data found in literature. The method developed can be well used for the separation of metallothionein isoforms and sub-isoforms.国家自然科学基金资助项目(No. 20175022);; 福建省重大科技项目(No. 2003Y005和No. 2003Y003)

Research on the Fluorescence Characteristics of Synechococcus sp.and Salt Algae

[目的]研究聚球藻和盐藻的荧光特性,确定其在特征激发、发射波长下藻浓度和荧光强度的关系,寻找一种确定藻类浓度的简便方法。[方法]以岛津rf5301型荧光分光光度计分析检测聚球藻和盐藻的激发和发射光谱,并获得它们的荧光强度与以血球计数板计数的藻浓度之间的关系。[结果]聚球藻和盐藻的激发、发射光谱有着明显的不同。在它们特征的激发、发射波长下,其浓度与荧光强度呈良好的线性关系。[结论]通过测定藻类的荧光强度就可推算出特定藻类的浓度,且该方法比血球计数板计算藻类的浓度更为便捷。[Objective] A simple determining method of the concentration of the known algae:Synechococcus sp.and salt algae,was formed through the confirmation of the relationship between its concentration and fluorescence intensity under its characteristics of excitation and emission wavelength based on research on its fluorescence characteristics.[Method] The excitation and emission spectra of Synechococcus sp.and salt algae was measured with the fluorescence spectrophotometer(RF5301) and the relationship between the fluorescence intensity and the concentration of alga based on the number at blood counting plate was gotten.[Results] There was a marked difference in the excitation and emission spectra between Synechococcus sp.and salt algae and there was good linear relationship between its concentration and the fluorescence intensity under its special excitation and emission wavelength.[Conclusion] The concentration of specific algae could be calculated through the determination of its fluorescence intensity,and the method was more convenient in the concentration-testing of algae than that of the blood cell counting sheet

Recent Development and Applications of Optical and Fiber-optic pH Sensors

本文综述了光纤化学 pH传感器的现状和发展 .分别从 pH指示剂的试剂固定化方法和传感信号的产生与检测方式来阐述近年来光纤化学pH传感器新技术的发展 ;同时也介绍了其他 pH传感器的发展现状 .This article provides a brief review on the development and applications of fiber optic pH sensors in recently years. Various methods and materials, different spectroscopic methods are introduced. Several special opticaland fiber optic pH sensors are reviewed.国家“8 63”科技攻关海洋领域 (818 0 9 0 7)资助项

Separation and Enrichment of Melamine in Feed by a New Molecular Imprinting Solid-phase Extraction Column

[目的]研制一种新型的分子印迹固相萃取小柱,用于分离富集饲料中的三聚氰胺。[方法]采用本体聚合法制备了三聚氰胺分子印迹聚合物,以该聚合物为填料制作三聚氰胺分子印迹固相萃取(MIP-SPE)小柱,优化了固相萃取条件,应用高效液相色谱(HPlC)法测定浓缩液中的三聚氰胺含量。[结果]自制的MIP-SPE小柱可以从饲料中选择性地分离、富集三聚氰胺,有效地去除饲料中的复杂基质,加标回收率约为95%。MIP-SPE小柱与空白印迹固相萃取小柱(nMIP-SPE)的对比试验表明,前者的萃取效率明显高于后者。[结论]自制的新型三聚氰胺MIP-SPE小柱可用于饲料提取液中的三聚氰胺高选择性分离富集,使用简便,具有广阔的应用前景。[Objective] The research aimed to develop a new molecular imprinting solid-phase extraction column for the separation and enrichment of melamine in feed.[Method] The molecular imprinting polymer of melamine was prepared by noumenon polymeric method.This polymer was used as filler to prepare molecular imprinting polymer solid-phase extraction(MIP-SPE) column of melamine.The solid-phase extraction conditions were optimized and melamine content in concentrated solution was determined by using HPLC.[Result]Melamine could be separated selectively from feed and enriched by home-made MIP-SPE column.It could wipe off complex matrix from feed and the addition recovery rate was 95%.The contrast experiment between MIP-SPE column and NMIP-SPE(non-imprinted polymer-solid phase extraction) column showed that the extraction efficiency of the former was obviously higher than the latter.[Conclusion] The home-made MIP-SPE column could be used to separate and enrich melamine in feed efficiently,with a broad application prospect.厦门市科技计划项目(3502Z20110018

STUDY OF PALLADIUM ANALYTE BINARY-SYSTEM IN THE GRAPHITE-FURNACE BY SURFACE ANALYTICAL TECHNIQUES

The mechanisms of the stabilization of Pb, Zn and As by a palladium modifier were investigated by scanning electron microscopy, X-ray diffraction spectrometry and X-ray photoelectron spectrometry. All three elements were found to form an intermetallic solid solution with excess of Pd. The concentration ratio of Pd to analyte varies with the surface depth of Pd-analyte species. Chemical shifts measured in the binding energy of Pd and analyte are insignificant. The monophase of the Pd lattice in which some Pd atoms are displaced by the analyte atoms has been identified as being dominant. It is suggested that the reduced Pd and analyte form a stable intermetallic solid solution during the ashing stage and the analyte atoms remain in the Pd lattice until the temperature is high enough to break down the lattice