福建沿海侨乡农村篮球运动开展现状与发展对策的研究

通过对福建沿海侨乡农村篮球运动开展现状的调查研究 ,既肯定其成绩又指出不足 ,同时提出一些发展对策 ,为我国广大农村开展篮球运动起到宣传和借鉴意义

我国中小体育用品生产企业产业集群集聚研究——以福建晋江运动鞋产业集群为实证

入世后,我国中小体育用品业面临着国外知名品牌企业的竞争威胁,引起了我国业内人士的高度重视;产业集聚战略已成为提升区域竞争力的重要措施之一。以晋江运动鞋行业为例证,分析了我国中小体育用品生产企业产业集群集聚竞争优势和形成条件

Multiresidue Determination of Organophosphorus Pesticide Residues in Vegetables and Fruit by Gas Chromatography-Negative Ion Chemical Ionization-Mass Spectrometry

将气相色谱-负离子化学电离质谱法(GC-NC I-M S)应用于蔬菜水果中9种有机磷农药残留的分析测定,初步解析了这些农药的NC I-M S特征阴离子结构和断裂机理,并初步探讨了GC-NC I-M S分析蔬菜水果中有机磷农药残留时基体效应的影响。采用空白样品基体匹配校准曲线法(M C)进行定量分析,有效地降低了基体效应的影响。蔬菜水果样品用乙酸乙酯超声提取,以乙硫磷为内标物,采用GC-NC I-M S的选择离子监测方式(S IM)进行定性和定量分析。9种有机磷农药的方法检测限为0.12~1.0μg/kg。在方法的检测限与1 000μg/kg范围内,线性相关系数都大于0.999 3。当空白蔬菜水果(西红柿)样品的加标水平为100,400,800μg/kg时,平均加标回收率为78%~126%,相对标准偏差为0.58%~14.7%。An analytical method of gas chromatography coupled with negative ion chemical ionization-mass spectrometry for simultaneous determination of nine organophosphorus pesticide residues in vegetables and fruit has been developed,and the negative ions structure and partition mechanism of the nine organophosphorus pesticides were interpreted.Meanwhile,the matrix effect for sample analysis was discussed,and matrix-matched calibration for quantification was introduced to reduce the matrix effect in this method.Pesticides were extracted from sample with ethyl acetate in an ultrasonic bath,then determined by gas chromatography-mass spectrometry operated in negative chemical ionization mode and quantified in selective ion monitoring mode,and ethion was used as an internal standard.The detection limits of the method were 0.12-1.0 μg/kg for the nine organophosphorus pesticides,and the relative coefficients were higher than(0.9993).A blank sample(tomato) was spiked at 100,400,800 μg/kg for each pesticide,and the recoveries were determined to be from 78% to 126% with relative standard deviations from 0.58% to 14.7% for the pesticides

Determination of Multiple Pesticide Residues in Honey Using Gas Chromatography-Mass Spectrometry

开展了蜂蜜中23种农药残留的气相色谱-电子轰击离子源质谱(GC-E I/M S)分析方法的研究,并对其中3种农药的E I/M S碎片离子的断裂机理与结构进行了初步解析。探讨了蜂蜜试样前处理条件的优化与选择。将蜂蜜试样用乙酸乙酯提取剂超声提取、F lo ris il硅藻土色谱柱净化和正己烷-乙酸乙酯(体积比为7∶3)混合洗脱剂洗脱后,以PCB103为内标物,采用选择离子监测(S IM)方式下的GC-E I/M S分析。当试样的加标浓度为50,100和200μg/kg时,加标回收率为82%~120%,相对标准偏差小于11.0%。23种农药的检测限都小于10.0μg/kg,线性范围为10~500μg/kg,相关系数都大于0.995。此分析方法已成功地应用于蜂蜜中23种痕量农药残留的分析。An analytical method was developed for the simultaneous determination of 23 pesticide residues in various commercial honeys.Meanwhile,the characteristic ions and fragmentation mechanism of three pesticides in the process of electron ionization mass spectrometry(EI/MS) were evaluated.After the optimization of different parameters such as the extraction solvent,pesticides were extracted from honey with ethyl acetate in an ultrasonic bath,cleaned up on a Florisil column by an elution of mixture of hexane and ethyl acetate(7∶ 3,v/v), and analyzed by gas chromatography-electron ionization mass spectrometry(GCEI/MS) in the selected ion monitoring mode(SIM) with PCB103 as internal standard.Recovery studies were performed at 50,100 and 200 μg/kg fortification levels for each pesticide,and the recoveries ranged from 82% to 120% with relative standard deviations between 1.8% and 11.0% for different pesticides.The limit of detection was less than 10.0 μg/kg for all the pesticides.The developed method was linear in the range of 10-500 μg/kg,with correlation coefficients larger than 0.995.Finally,the developed analytical method has been successfully applied to the determination of pesticide residues in several honey samples

围生期窒息新生儿血清IL-6 、sICAM-1 水平的动态变化及其临床意义

【目的】了解围生期窒息新生儿血清IL-6 、sICAM-1 水平的动态变化。【方法】采用双抗体夹心ELISA 方法, 检 测41 例围生期窒息新生儿及11 例正常新生儿生后出生时、第3 天、第7 天血清IL-6、sICAM-1 的水平。【结果】41 例围生期 窒息新生儿中26 例合并缺氧缺血性脑病, 其中轻度12 例, 中度8 例, 重度6 例。对照组血清IL-6 的水平生后1 周内无明显 变化, 缺氧缺血性脑病(HIE)组血清IL-6 水平呈先升后降的趋势:生后第3 天达高峰, 第7 天下降, 较出生时水平低, 随着 HIE 程度的加重, IL-6 水平呈上升趋势。对照组血清sICAM-1 水平随日龄增加呈上升趋势, 重度HIE 组各天的水平均显著高 于对照组、单纯窒息组及轻度、中度HIE 组各天的水平(P <0.05 或0.01), 其余4 组间各天的水平差异无显著性。围生期窒息 新生儿的血清IL-6 水平与血清sICAM-1 水平无相关关系。【结论】血清IL-6 、sICAM-1 水平与脑损伤的程度及预后密切相关

Multiresidue Determination of 17 Organochlorine and Pyrethroid Pesticides in Tea by Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry

建立了茶叶试样中17种农药残留(8种有机氯和9种拟除虫菊酯农药)的气相色谱-负化学离子源-质谱(GC-NC I-MS)联用的分析方法.茶叶试样用V(正己烷)/V(丙酮)=1/1混合提取剂超声提取,经F lorisil硅藻土和中性氧化铝混合层析柱净化后,以环氧七氯为内标物,采用GC-NC I-MS的选择离子监测方式(SIM)分析;探讨了茶叶试样的基体诱导色谱响应增强影响所产生的分析误差及其减小的措施,用空白试样基体匹配校准曲线法(MC法)定量分析.当加标质量浓度水平为20,50和200μg/kg时,加标回收率为67.9%~129%,相对标准偏差为1.0%~20%,除氯菊酯农药的检出限为8.3μg/kg外,其余大部分农药的检出限均小于1.0μg/kg,线性范围为10~500μg/kg,相关系数均大于0.996,此方法成功地应用于茶叶试样中痕量农药残留的分析.An analytical multiresidue method for the simultaneous determination of 17 pesticides(8 organochlorines and 9 pyrethroids) in tea was developed.Pesticides were extracted from tea with hexane-acetone(volume ratio is 1∶1) in an ultrasonic bath and cleaned up on a Florisil and neutral alumina column, then were determined by gas chromatography with negative chemical ionization mass spectrometric detection in the selected ion monitoring mode,and with heptachlor epoxide as the internal standard.Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination.The recovery studies were performed at 20,50 and 200 μg/kg fortification levels for each pesticide,and the recoveries ranged from 67.9% to 129% with a relative standard deviation between 1.0% and 20% for the different pesticides. The detection limit of the method was less than 1.0 μg/kg for most of pesticides except for the permethrin.The developed method was linear over the range assayed,10-500 μg/L,with determination coefficients>0.996.Finally,the developed analytical method was successfully applied to the determination of pesticides in several tea samples

Multiresidue determination of organochlorine pesticides in honey by gas chromatography-mass spectrometry

建立了气相色谱-电子轰击离子化-质谱法(GC-EI-MS)同时分析蜂蜜试样中12种有机氯农药残留的分析方法。蜂蜜试样用V(正己烷)∶V(乙酸乙酯)=5∶1混合提取剂超声提取和Florisil硅藻土层析柱净化后,以PCB 103为内标物,采用GC-EI-MS的选择离子监测方式(SIM)分析,同时探讨了一些有机氯农药EI-MS特征离子的结构与断裂机理。当空白试样的加标浓度为10、50、200μg/kg时,加标回收率为80%~112%,相对标准偏差为0.4%~9.8%,方法检出限为0.2~4.0μg/kg,其中8种农药的MDL0.996.Finally,the developed analytical method has been successfully applied to the determination of pesticides in several honey samples

Multiresidue determination of pyrethroid pesticides in fruit juices by matrix solid-phase dispersion and gas chromatography-negative chemical ionization-mass spectrometry

建立了基质固相分散法(MSPD)和气相色谱-负化学离子源-质谱法(GC-NCI-MS)应用于果汁中10种拟除虫菊酯农药残留量的快速分析方法,并对这些农药NCI-MS的阴离子结构与断裂机理进行初步探讨。采用以中性氧化铝为吸附剂、Florisil硅藻土为净化剂和乙酸乙酯为洗脱剂的MSPD样品前处理方法,以PCB103为内标物和GC-NCI-MS的选择离子监测方式(SIM)进行定性与定量分析。当样品的加标浓度水平为50、250μg/kg时,平均加标回收率为86.7%~114.8%,相对标准偏差为1.9%~14.1%;除氯菊酯农药的方法检出限(MDL)为14.7μg/kg外,其余农药的MDL大都小于1.0μg/kg;线性范围为10~500μg/kg,相关系数都大于0.997,在所分析的大部分果汁中至少分析出两种以上的拟除虫菊酯农药残留。A rapid method based on matrix solid-phase dispersion was developed for the determination of ten pyrethroid pesticides in commercial juices.Meanwhile,negative ion structure and fracture mechanism of these pesticides of negative chemical ionization mass spectrometry were evaluated.The group of pesticides was added to juice and blended with neutral alumina,the mixture was packed into disposable filtration column,this column was tandem with florisil as cleaning and was eluted with ethyl acetate.The analysis of samples was accomplished using gas chromatography with negative chemical ionization mass spectrometric detection(GC-NCIMS) in the selected ion monitoring mode(SIM),and with PCB103 as internal standard.Recovery studies were performed at 50 and 250 μg/kg fortification levels for each pesticide,and the average recoveries ranged from 86.7 to 114.8% with a relative standard deviation between 1.9% and 14.1% for the different pesticides. The detection limit of the method was less than 1.0 μg/kg for most of pesticides except for the permethrin.The developed method was linear over the range assayed,10～500μg/kg,with correlation coefficients >0.997.The proposed method was applied to the analysis of these compounds in commercial juice samples.At least two pesticides was found in most of the samples

大气污染物监测数据不确定度评估方法体系建立及其对PMF源解析的影响分析

目前，正定矩阵因子法（ＰＭＦ）在大气污染物来源解析中得到了广泛应用，而监测数据不确定度评估是 ＰＭＦ 源解析的重要内容之一．当前 绝大部分研究采用的数据不确定度仅通过借鉴前人的方法简单计算而得，缺乏对计算方法的合理性和适用性进行评估．本研究通过 ３ 种常用 的不确定度算法交互应用建立了一套有效评估不确定度的方法体系．通过对香港荃湾站点 １９９８—２００８ 年 ＰＭ１０组分监测数据进行源解析并与 平行采样数据源解析结果进行对比，对该方法体系的合理性进行了验证．结果发现，应用该方法体系可以将某些常规方法无法分离的因子进一 步分解，得到的源解析结果的残差值甚至小于平行采样方法解析结果的残差值，得到的因子贡献率均处于常规方法得出的因子贡献率之间．这 些均表明了该方法体系所得源解析结果的可靠性和全面性．因此，本研究建立的评估不确定度的方法体系具有较强的可行性，对确保源解析结 果的准确性有重要意义．Positive matrix factorization (PMF) has been applied extensively in source apportionment of atmospheric pollutants. Data uncertainty is one of the most important input information for PMF analysis. Currently, data uncertainty is calculated by some simple formulae referenced from previous studies, lacking evaluation of their reasonableness and applicability. In this study, we develop an uncertainty assessment framework (UAF) by utilizing three common uncertainty calculation algorithms. The effectiveness of this UAF is assessed by comparing with the source apportionment results on parallel measurement of PM 10 compositions at Tsuen Wan station in Hong Kong during 1998-2008. It is found that applying UAF could further decompose some factors which couldn't by traditional methods. The derived scaled residuals are even smaller than those from source apportionment on parallel measurement. Source contributions derived by UAF are well in between those from traditional methods. All above indicates the reliability and completeness of source apportionment by UAF. It is thus concluded that this UAF has great applicability and usefulness in ensuring the accuracy of source apportionment results. © 2019, Science Press. All right reserved

THE SIMULTANEOUS DETERMINATION OF SUDAN Ⅰ AND SUDAN Ⅱ BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY IN FOODSTUFFS

将气相色谱-电子轰击离子源-质谱法(GC-EI-MS)应用于番茄沙司和辣椒酱中苏丹Ⅰ和苏丹Ⅱ添加剂的同时分析,并对两种化合物的EI-MS主要碎片离子的结构与断裂机理进行初步解析.分析方法的线性范围为24—800μg.kg-1,相关系数(R2)均大于0.993,相对标准偏差(RSD)均小于12.7%,样品的加标回收率为77.3%—106%,苏丹Ⅰ的方法检出限(LOQ)为7.8μg.kg-1,苏丹Ⅱ的LOQ为6.8μg.kg-1.Gas chromatography-mass spectrometer equipped with election impact ionization source(GC-EI-MS)was put forward for the determination of Sudan Ⅰ and Sudan Ⅱ in foodstuffs.The faulted mechanisms of the fragment ions and the structures of them of Sudan Ⅰ and Sudan Ⅱ under election impact ionization were parsed.The linear range of the method was 25—800 μg·kg~(-1) and the square correlation coefficients(R~2) was lager than 0.993.The relative standard deviation(RSD) of the method was lower than 12.7%.The recovery values ranged from 77.3% to 106%.The limit of quantifacation(LOQ) was 7.8 μg·kg~(-1) for Sudan Ⅰ and 6.8(μg·kg)~(-1) for Sudan Ⅱ