A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 pol...A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 polycyclic aromatic hydrocarbons(PAHs),70 polychlorinated biphenyls(PCBs),123 pesticides,20 phthalate esters(PAEs),4 organophosphate esters(OPEs),9 synthetic musks(SMs),and 5 UV filters(UVs)in water.No-tably,this method provided a decent linearity of calibration standards(R^(2)>0.999),excellent method limits of quantification(MLOQs)(0.12–11.41 ng/L),satisfactory matrix spiking recovery rates(60.4%–126%),and high precision(intra-day relative standard deviations(RSDs):1.0%–10.0%,inter-day RSDs:3.0%–15.0%,and inter-week RSDs:3.4%–15.7%),making it suitable for trace-level studies.Statistical analysis revealed that SVOCs with higher volatility exhibited enhanced recovery rates.Validation of the methodology involved analyzing SVOCs in real spring water and river water samples.Twenty-seven SVOCs were detected in spring water and 58 in river water,with an average concentration of 631.73 and 16,095 ng/L,respectively.Among the detected SVOCs,PAEs constituted the predominant proportion.This study underscored the presence of SVOCs contamination specifi-cally within the spring water,although SVOCs concentrations in river water were significantly greater than those found in spring water.In summary,this sensitive method based on SPE–GC–MS/MS was successfully developed and validated for the rapid analysis of a diverse array of 256 SVOCs at trace levels in water,including not only the traditional highly valued PAHs,PCBs,pesticides,and PAEs,but also the emerging OPEs,UVs,and SMs.展开更多
本文建立同时检测3种4(3H)-喹唑啉酮滥用物质甲喹酮、依他喹酮和甲氧喹酮的GC-MS与GCMS/MS分析方法,并分别应用于实际案件中对疑似毒品与滥用人员毛发进行分析。使用选择离子监测模式(selected ion monitoring,SIM)和多反应监测模式(mul...本文建立同时检测3种4(3H)-喹唑啉酮滥用物质甲喹酮、依他喹酮和甲氧喹酮的GC-MS与GCMS/MS分析方法,并分别应用于实际案件中对疑似毒品与滥用人员毛发进行分析。使用选择离子监测模式(selected ion monitoring,SIM)和多反应监测模式(multiple reaction monitoring,MRM)分别对甲喹酮、依他喹酮和甲氧喹酮的标准品溶液进行分析,确定三种物质的特征碎片离子和特征离子对,并利用所建立的两种方法分别对实际案例中的疑似毒品和毛发样本进行检验。建立的GC-MS分析方法在送检的疑似毒品中检出甲喹酮、依他喹酮和甲氧喹酮成分且含量分别为11、4.3、2.5μg/mg,建立的GC-MS/MS分析方法在送检的毛发中检出甲喹酮、依他喹酮和甲氧喹酮成分且含量分别为148 ng/mg、565 pg/mg、58.2 ng/mg。本研究建立的GC-MS及GC-MS/MS检测方法具有简单、快速、准确的特点,可为疑似毒品与滥用人员毛发中甲喹酮、依他喹酮和甲氧喹酮的检测提供可靠的科学依据。展开更多
建立气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)测定鲜蛋中五氯酚钠残留量的方法。本文通过特定前处理步骤净化干扰物,采用乙酸酐-吡啶溶液衍生化,GCMS/MS检测,内标法定量。结果显示,该方法线性良好,回...建立气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)测定鲜蛋中五氯酚钠残留量的方法。本文通过特定前处理步骤净化干扰物,采用乙酸酐-吡啶溶液衍生化,GCMS/MS检测,内标法定量。结果显示,该方法线性良好,回收率为86%~106%,相对标准偏差为3.3%~8.3%,定量限可达0.2μg·kg^(-1),较现有国家标准方法更灵敏,能满足蛋类食品日常检测需求。展开更多
目的建立一种同时测定尿液中麻黄碱(Ephedrine)和伪麻黄碱(Pseudoephedrine)成分的气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)分析方法。方法用乙酸乙酯提取含有麻黄碱和伪麻黄碱成分的尿液,离心取上清...目的建立一种同时测定尿液中麻黄碱(Ephedrine)和伪麻黄碱(Pseudoephedrine)成分的气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)分析方法。方法用乙酸乙酯提取含有麻黄碱和伪麻黄碱成分的尿液,离心取上清后氮吹挥干后用七氟丁酸酐60μL 70℃衍生化30 min后,再氮吹挥干后用50μL甲醇溶解后,进行GC-MS/MS分析。结果用本方法检测尿液中麻黄碱在0.05~10μg/mL;伪麻黄碱在0.02~5μg/mL范围内有良好的线性关系,相关系数为分别为0.9998、0.9995,提取回收率分别为89.4%~95.8%、90.3%~93.8%;两者的检测限和定量限分别为0.005μg/mL、0.01μg/mL,日内精密度和准确度分别<5.87%、9.56%,日间精密度和准确度分别<7.54%、9.27%,室温和-20℃条件下,尿液中麻黄碱和伪麻黄碱在15 d内具有良好的稳定性。结论本研究建立的尿液中麻黄碱和伪麻黄碱成分的GC-MS/MS分析方法,准确、稳定、灵敏,可以为苯丙胺类毒品或者卡西酮类新精神活性药物的法医毒物分析提供可靠的数据和方法学支持。展开更多
基金supported by the National Natural Science Foundation of China(No.51939009)Shenzhen Science and Technology Program(Nos.JCYJ20241202125905008 and GXWD20201231165807007-20200810165349001).
文摘A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 polycyclic aromatic hydrocarbons(PAHs),70 polychlorinated biphenyls(PCBs),123 pesticides,20 phthalate esters(PAEs),4 organophosphate esters(OPEs),9 synthetic musks(SMs),and 5 UV filters(UVs)in water.No-tably,this method provided a decent linearity of calibration standards(R^(2)>0.999),excellent method limits of quantification(MLOQs)(0.12–11.41 ng/L),satisfactory matrix spiking recovery rates(60.4%–126%),and high precision(intra-day relative standard deviations(RSDs):1.0%–10.0%,inter-day RSDs:3.0%–15.0%,and inter-week RSDs:3.4%–15.7%),making it suitable for trace-level studies.Statistical analysis revealed that SVOCs with higher volatility exhibited enhanced recovery rates.Validation of the methodology involved analyzing SVOCs in real spring water and river water samples.Twenty-seven SVOCs were detected in spring water and 58 in river water,with an average concentration of 631.73 and 16,095 ng/L,respectively.Among the detected SVOCs,PAEs constituted the predominant proportion.This study underscored the presence of SVOCs contamination specifi-cally within the spring water,although SVOCs concentrations in river water were significantly greater than those found in spring water.In summary,this sensitive method based on SPE–GC–MS/MS was successfully developed and validated for the rapid analysis of a diverse array of 256 SVOCs at trace levels in water,including not only the traditional highly valued PAHs,PCBs,pesticides,and PAEs,but also the emerging OPEs,UVs,and SMs.
文摘建立气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)测定鲜蛋中五氯酚钠残留量的方法。本文通过特定前处理步骤净化干扰物,采用乙酸酐-吡啶溶液衍生化,GCMS/MS检测,内标法定量。结果显示,该方法线性良好,回收率为86%~106%,相对标准偏差为3.3%~8.3%,定量限可达0.2μg·kg^(-1),较现有国家标准方法更灵敏,能满足蛋类食品日常检测需求。
