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Validation of a Method for Characterization of Ethanol in Water by HS-GC-FID to Serve the Traceability of Halal Measurements
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作者 Adel B. Shehata Abdulrahman R. Al Askar +3 位作者 Mohammed A. Al Rasheed Abdulrahman M. Al Zahrany Fahd A. Al Kharraa Sowailem A. Al Sowailem 《Green and Sustainable Chemistry》 2024年第2期17-28,共12页
The determination of the ethanol content in food products is of fundamental importance for HALAL certification. In this work, an analytical method for the determination of ethanol in water by headspace gas chromatogra... The determination of the ethanol content in food products is of fundamental importance for HALAL certification. In this work, an analytical method for the determination of ethanol in water by headspace gas chromatography with flame ionization detector (HS-GC-FID) has been developed and validated for the use in characterization of ethanol reference materials. The validation study was carried out in the linear calibration range 100 - 1500 mg/kg using the NIST SRM 2900, nominal 95.6%. The studied performance characteristics of the method were the limit of detection, LOD, the limit of quantification LOQ, selectivity, linearity, precision, recovery and bias. The validation results showed that the method is selective, precise, accurate and free from any significant bias. The LOD and LOQ were 1.27 and 3.86 mg/kg respectively and the estimated expanded uncertainty was 2% indicating that the method is fit for the purpose of certification of ethanol in water reference materials. 展开更多
关键词 ETHANOL hs-gc-fid VALIDATION LINEARITY Precision Bias
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HS-GC-FID测定纺织品中DMF和DMAC 被引量:3
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作者 郭奕辰 王麟 +1 位作者 曹石淼 程弯 《印染》 北大核心 2016年第8期44-48,共5页
建立顶空气相色谱法同时测定纺织品中N,N-二甲基甲酰胺(DMF)和N,N-二甲基乙酰胺(DMAC)残留量的方法。将样品置于顶空进样器中平衡,供气相色谱检测,使用CD-WAX色谱柱进行分离,以氢火焰离子化检测器(FID)进行测定,外标法定量。优化... 建立顶空气相色谱法同时测定纺织品中N,N-二甲基甲酰胺(DMF)和N,N-二甲基乙酰胺(DMAC)残留量的方法。将样品置于顶空进样器中平衡,供气相色谱检测,使用CD-WAX色谱柱进行分离,以氢火焰离子化检测器(FID)进行测定,外标法定量。优化顶空条件和气相色谱条件,使DMF与DMAC在色谱图中具有良好的峰响应。DMF与DMAC的加标回收率在80.54%-96.83%,精密度为2.42%-8.81%,检出限分别为0.09 mg/kg和0.15 mg/kg。 展开更多
关键词 测试 DMF DMAC 顶空气相色谱法 fid检测器 纺织品
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HS-GC-FID法测定豆粕中6种溶剂残留
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作者 张静 周秀锦 +2 位作者 邵宏宏 张晓玲 晁铎源 《分析仪器》 CAS 2019年第1期141-145,共5页
建立了顶空-气相色谱-氢火焰离子化检测法(HS-GC-FID)测定豆粕中6种烷烃类残留溶剂的新方法。豆粕样品经80℃振荡平衡30min后即可进样分析,采用Rxi-5Sil MS毛细管柱分离,FID测定,外标法定量。结果表明,6种目标分析物在0.2~10.0mg/kg间... 建立了顶空-气相色谱-氢火焰离子化检测法(HS-GC-FID)测定豆粕中6种烷烃类残留溶剂的新方法。豆粕样品经80℃振荡平衡30min后即可进样分析,采用Rxi-5Sil MS毛细管柱分离,FID测定,外标法定量。结果表明,6种目标分析物在0.2~10.0mg/kg间均呈现良好线性关系,相关系数(R2)大于0.990,方法检测限(LOD)0.075mg/kg,定量限(LOQ)0.2mg/kg,平均加标回收率95.3%~106.3%,相对标准偏差(RSD)小于8.3%。该方法操作简单且灵敏度高,可满足豆粕中残留溶剂的日常检测需要。 展开更多
关键词 hs-gc-fid 残留溶剂 豆粕
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基于静态模型的五种苯系物在海水和厚壳贻贝中的消除规律
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作者 宋立玲 周旭 +3 位作者 廖思扬 於佩佩 胡芬静 周秀锦 《湖北农业科学》 2023年第6期29-32,共4页
对静态模型中的苯(BZ)、甲苯(TU)、对二甲苯(PX)、邻二甲苯(MX)和间二甲苯(OX)5种苯系物在海水和厚壳贻贝(Mytilus coruscus)中的消除规律进行研究,在(20±0.5)℃环境温度下,以海水和厚壳贻贝为研究对象,分别添加一定浓度的5种苯系... 对静态模型中的苯(BZ)、甲苯(TU)、对二甲苯(PX)、邻二甲苯(MX)和间二甲苯(OX)5种苯系物在海水和厚壳贻贝(Mytilus coruscus)中的消除规律进行研究,在(20±0.5)℃环境温度下,以海水和厚壳贻贝为研究对象,分别添加一定浓度的5种苯系物,用顶空进样-气相色谱氢火焰离子化检测器法(HS-GCFID)分析不同时间点的5种苯系物在海水和厚壳贻贝中的残留浓度。结果表明,海水和厚壳贻贝中苯系物各组分浓度随时间变化规律基本相同,海水中5种苯系物的消除速率由大到小依次为MX、PX、TU、BZ、OX,厚壳贻贝中5种苯系物的消除速率由大到小依次为TU、BZ、MX、OX、PX,厚壳贻贝与海水的消除速率不同,其原因可能是厚壳贻贝富含脂肪、蛋白质等复杂基质,苯系物与厚壳贻贝基质的结合程度较强。 展开更多
关键词 hs-gc-fid 苯系物 海水 厚壳贻贝(Mytilus coruscus)
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顶空气相色谱法测定玉米中的乙烯利残留 被引量:7
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作者 黄玉婷 邵华 +5 位作者 杨丽华 李敏杰 杜欣蔚 金茂俊 金芬 王静 《食品工业科技》 CAS CSCD 北大核心 2012年第22期78-80,共3页
利用顶空-气相色谱-氢火焰离子化分析方法(HS-GC-FID)对玉米中乙烯利残留量进行了测定,并分析了不同顶空和色谱条件对玉米中乙烯利残留测定的影响,建立了玉米中乙烯利残留量的顶空-气相色谱检测方法。玉米样品经甲醇提取、离心、浓缩,采... 利用顶空-气相色谱-氢火焰离子化分析方法(HS-GC-FID)对玉米中乙烯利残留量进行了测定,并分析了不同顶空和色谱条件对玉米中乙烯利残留测定的影响,建立了玉米中乙烯利残留量的顶空-气相色谱检测方法。玉米样品经甲醇提取、离心、浓缩,采用HS-GC-FID法测定其中乙烯利含量。方法的线性相关系数为0.9999,相对标准偏差为1.07%~5.70%,样品加标回收率为72.01%~90.85%,方法的最低检出限为0.1mg/kg。该方法简单、易操作,适于玉米中乙烯利的定量分析。 展开更多
关键词 玉米 乙烯利 顶空气相色谱法
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优化GC检测欧李酒香气成分的萃取条件 被引量:13
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作者 陈臣 李艳 牟德华 《食品工业科技》 CAS CSCD 北大核心 2014年第6期81-86,共6页
香气物质的组成表征果酒的特色,利用响应面法优化顶空固相微萃取(HS-SPME)欧李果酒中香气物质的条件,使气相色谱法检测香气物质的结果更精确。本文采用HS-SPME结合GC-FID检测欧李发酵酒中的香气物质,在单因素实验的基础上,以加盐量、萃... 香气物质的组成表征果酒的特色,利用响应面法优化顶空固相微萃取(HS-SPME)欧李果酒中香气物质的条件,使气相色谱法检测香气物质的结果更精确。本文采用HS-SPME结合GC-FID检测欧李发酵酒中的香气物质,在单因素实验的基础上,以加盐量、萃取温度、萃取时间为影响因素,出峰面积为响应值,运用Box-Benhnken中心组合实验设计原理进行响应面分析,优化了HS-SPME的萃取条件。结果表明,HS-SPME萃取欧李发酵酒中香气成分的适宜条件为:加盐量0.226g/mL、萃取温度29℃、萃取时间36min。该条件下萃取,结合GC-FID测得欧李发酵酒中32种香气成分,对其中10种进行了定性和定量分析,含量较高的有:异戊醇110.734mg/L、己酸乙酯11.568mg/L、异丁醇8.7725mg/L、苯乙醇47.178mg/L、乙酸异戊酯15.655mg/L、丙醇1.7032mg/L。 展开更多
关键词 HS—SPME 响应面优化 GC—fid 欧李发酵酒 香气成分
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顶空固相微萃取-气要色谱-氢火焰离子化法检测啤酒中的酒花香气成分 被引量:1
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作者 江伟 孙志伟 +3 位作者 刘伟成 刘敬忠 李桂玲 任广鹏 《啤酒科技》 2009年第8期23-26,共4页
来自酒花的微量香气成分会影响啤酒的感官评价和质量。为评价酒花香气对啤酒的影响,本文采用顶空固相微萃取(Hs—SPME)对啤酒前处理后,使用常见且低成本维护的气相色谱一氢火焰离子化法fGC—FID)进行定性定量。以2一壬醇为内标,... 来自酒花的微量香气成分会影响啤酒的感官评价和质量。为评价酒花香气对啤酒的影响,本文采用顶空固相微萃取(Hs—SPME)对啤酒前处理后,使用常见且低成本维护的气相色谱一氢火焰离子化法fGC—FID)进行定性定量。以2一壬醇为内标,测定出里那醇、乙酸香茅酯、仪一萜品醇、B一香茅醇、香叶醇5种酒花香气成分。此法的精密度为4.69%~13.41%,回收率为74.95%~106.09%,检出限为0.005~O.028μg·L-1。通过此法进行啤酒检测,结果显示:啤酒中这5种酒花香气含量均〈10μg·L-1,大部分在0.10~5.00μg·L-1之间。研究表明:该法测定准确可靠;与已有方法如顶空固相微萃取一气质联用法(HS—SPME—GC—Ms)相比,该法的仪器常见,维护成本更低,更适合啤酒厂推广使用。 展开更多
关键词 啤酒 酒花 HS-SPME GC-fid 微量成分 萜类化合物 气相色谱-质谱法(GC-MS)
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非正常死亡案件中丙酮含量分析
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作者 宋丽娟 赵培铎 张广华 《刑事技术》 2015年第3期256-258,共3页
目的利用顶空气相色谱分离分析方法,在无法实施尸体解剖时,通过测定血液或尿液中丙酮的含量为某些非正常死亡案件提供死因判定的依据。方法利用丙酮易挥发性,用顶空气相色谱/氢火焰离子化检测器(HSGC/FID)进行分离检测;通过与平行操作... 目的利用顶空气相色谱分离分析方法,在无法实施尸体解剖时,通过测定血液或尿液中丙酮的含量为某些非正常死亡案件提供死因判定的依据。方法利用丙酮易挥发性,用顶空气相色谱/氢火焰离子化检测器(HSGC/FID)进行分离检测;通过与平行操作的对照品比较,以保留时间为依据进行定性分析;以峰面积为依据,采用内标法(叔丁醇作为内标物)进行定量测定。结果通过对死者血液和尿液测定,分析丙酮含量异常数据,同时结合前期调查所获取的案件相关信息,为死因判定提供了依据。结论该分析方法基质干扰小,重现性良好,操作简单,普通刑事化验室均可进行,对缺乏病理学数据的非正常死亡案件的死因判定具有重要意义。 展开更多
关键词 法医毒物学 非正常死亡 顶空气相色谱/氢火焰离子化检测器 血液 尿液 丙酮
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HS-GC-FID法检测海产品中的二甲苯 被引量:1
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作者 周秀锦 邵宏宏 +4 位作者 张静 顾海刚 晁铎源 陈瑶 韩超 《分析试验室》 CAS CSCD 北大核心 2018年第8期906-909,共4页
建立了顶空进样-气相色谱氢火焰离子化检测器法(HS-GC-FID)检测海产品中的3种二甲苯同分异构体。海产品经过90℃温育和振荡平衡40 min顶空进样,HP-INNOWAX毛细管柱分离,程序升温,FID检测,外标法定量。结果表明,3种二甲苯同分异构体在0.1... 建立了顶空进样-气相色谱氢火焰离子化检测器法(HS-GC-FID)检测海产品中的3种二甲苯同分异构体。海产品经过90℃温育和振荡平衡40 min顶空进样,HP-INNOWAX毛细管柱分离,程序升温,FID检测,外标法定量。结果表明,3种二甲苯同分异构体在0.1~1.0 mg/kg的浓度范围内呈线性,相关系数均在0.99以上,方法检出限为0.035 mg/kg,定量限为0.1 mg/kg,平均回收率在87.7%~112.9%之间,相对标准偏差(RSD)小于10.9%。该法具有操作简单、能够准确定性、灵敏度较高的特点,适合海产品中二甲苯残留量的测定。 展开更多
关键词 hs-gc-fid 二甲苯 海产品
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Optimization of Headspace Solid-Phase Microextraction Conditions for the Identification of Volatiles Compounds from the Whole Fruit of Lemon, Lime, Mandarin and Orange
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作者 Khalid Mohammed Manjree Agarwal +1 位作者 James Newman Yonglin Ren 《Journal of Biosciences and Medicines》 2017年第3期176-186,共11页
An optimum method has been developed for extracting volatile organic compounds (VOCs) which contribute to the aroma of different species of citrus fruit (orange, lemon, lime, and mandarin). Headspace solid phase micro... An optimum method has been developed for extracting volatile organic compounds (VOCs) which contribute to the aroma of different species of citrus fruit (orange, lemon, lime, and mandarin). Headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled with flame ionization detection (FID) is used as a very simple, efficient and non-destructive extraction method. A three phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing time for volatiles reaching equilibrium from whole fruit in the headspace of the chamber was 20, 16, 8 and 16 hours for lemon, lime, mandarin, and orange respectively. Optimum fibre exposure times for whole fruit were 2, 4, 2 and 2 hours for lemon, lime, mandarin, and orange respectively. Three chamber volumes (500, 1000 and 2000 ml) were evaluated for the collection of VOCs with the 500 ml chamber being selected. The 500ml chamber produced the highest quality peak areas and quantity of extracted volatiles. As a result of fruit respiration, the percentage of oxygen (O2) of all citrus fruit species in 500 ml chamber decreased from 21.8% to 18.8% in the 20 hours sealing time, while carbon dioxide (CO2) contents increased to 2.9% also in the 20 hours sealing time. The results of this study showed the feasibility of this technique for identifying VOCs from four of the citrus fruit species and its potential as a routine method for physiological studies on citrus fruit or on other fruit species. 展开更多
关键词 Citrus FRUITS VOCs HS-SPME/GC-fid LEMON LIME MANDARIN ORANGE
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Safety of Lebanese Bottled Waters: VOCs Analysis and Migration Studies
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作者 Aline Ghanem Jacqueline Maalouly +2 位作者 Roula Abi Saad Dalia Salameh Chawki Oscar Saliba 《American Journal of Analytical Chemistry》 2013年第4期176-189,共14页
Despite the worldwide increase in the consumption of PET-bottled mineral waters compared to tap waters encouraged by its microbiological and chemical safety for public health, contaminants could migrate from the plast... Despite the worldwide increase in the consumption of PET-bottled mineral waters compared to tap waters encouraged by its microbiological and chemical safety for public health, contaminants could migrate from the plastic packaging into the water and induce adverse effects on human health. Volatile organic compounds (VOCs), including benzene, toluene, ethylbenzene, ortho, meta, and para-xylenes (BTEX), styrene, chlorobenzene and benzaldehyde are among the potential contaminants of bottled waters. This study aimed to assess Lebanese PET-bottled waters, in respect of VOCs contents, with comparison to polycarbonate-bottled and tap waters. Both HS-SPME-GC/FID and SPE-GC/FID were optimized and validated for VOCs determination in the waters, and their performances were compared. The HS-SPME-GC/FID was valid (Afnor NF T 90-210 (May 2009)) for all the studied molecules with limits of quantifications (LOQ) far lower the maximum contaminants levels (MCLs) set by both US-EPA and WHO. SPE-GC/FID was valid only for ethylbenzene, m/p-xylenes, o-xylene, and styrene, with poorer LOQs. HS-SPME-GC/FID was used therefore for VOCs monitoring in studied water samples showing the safety of the Lebanese bottled-water. The effects of bottles storage conditions (time, and exposure to sunlight) on VOCs migration were also studied. 展开更多
关键词 BTEX STYRENE HS-SPME-GC/fid SPE-GC/fid
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Screening for volatile sulphur compounds in a fatal accident case 被引量:1
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作者 Ping Xiang Huosheng Qiang +1 位作者 Baohua Shen Min Shen 《Forensic Sciences Research》 2017年第4期192-197,共6页
Acute fatal poisoning due to the inhalation of toxic gas frequently occurs in China.Volatile sulphur compounds(VSCs)are toxic to humans.In fatal poisoning investigations,such as those in industrial settings,a number o... Acute fatal poisoning due to the inhalation of toxic gas frequently occurs in China.Volatile sulphur compounds(VSCs)are toxic to humans.In fatal poisoning investigations,such as those in industrial settings,a number of VSCs,including methanethiol(MT),dimethyl sulphide(DMS),dimethyl disulphide(DMDS)and dimethyl trisulphide(DMTS),can coexist.To date,there is limited data regarding these compounds in post-mortem cases.In the present study,we report toxicological findings in a fatal accident case with two victims.Headspace gas chromatography/flame ionization detector with two columns of different polarities was utilized to screen MT,DMS,DMDS and DMTS in blood.The limits of detection in both methods were 0.05 mg/mL.No sulphur compounds were detected in the blood samples of the two victims.DMS and DMDS were detected in the lungs at concentrations of 0.5 and 1.3 mg/g and 2.2 and 4.1 mg/g,respectively.DMDS liver concentrations were 2.5 and 6.5 mg/g.In addition to hydrogen sulphide,screening for additional VSCs could help establish the cause of death. 展开更多
关键词 Forensic science forensic toxicology volatile sulphur compounds hs-gc/fid SCREENING fatal accident case
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