早期湿疹婴儿的气质特征研究

目的研究早期湿疹婴儿气质因子水平与分型特征，为湿疹婴儿的早期干预提供依据。方法采用1：2配比的回顾性病例对照研究，应用国内标化的小婴儿气质问卷（EITQ），对1月龄湿疹婴儿56例及112例正常婴儿进行气质因子水平及气质类型测评并比较。结果湿疹组与对照组气质类型总体分布比较，湿疹组男婴D型和I-D型明显高于对照组，E型和I-E型显著低于对照组（P＜0.001）；气质维度的单因素条件Logistic回归分析显示婴儿湿疹气质的影响因素有婴儿活动水平、节律性、适应性和反应强度四个维度（P＜0.05）；进一步气质维度的多因素条件Logistic回归分析（向后法）显示，适应性和反应强度两个维度为独立影响因素，湿疹组婴儿适应性较强、反应强度较弱。结论早期湿疹婴儿适应性较强、反应强度较弱，应根据其气质特征进行早期干预

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

中国人名地名的韩语标记教学探析

依据韩国《外来词标记法》第四章第二节的规定，中国人名地名的韩语标记采用原地音化与汉字音化并行，这一规定造成了中国人名地名的韩语标记多种多样，没有统一的准则。论文结合目前中国4年制本科院校韩国语专业普遍使用的教材《大学韩国语》1-4册中的中国人名地名韩语标记实例，分析目前韩国语学习中人名地名韩语标记的不足，探析人名地名韩语标记的正确范式。</jats:p

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

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

Multiresidue determination of 17 organochlorine and pyrethroid pesticides in tea by gas chromatography-negative chemical ionization-mass spectrometry

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 mu g/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 mu g/kg for most of pesticides except for the permethrin. The developed method was linear over the range assayed, 10-500 mu g/L, with determination coefficients > 0.996. Finally, the developed analytical method was successfully applied to the determination of pesticides in several tea samples