Ping Wang, Zhong-Min Wang, Jeff Wagner, Kazukiyo Kumagai
{"title":"建立了无溶剂热解吸-气相色谱-串联质谱法(TD-GC-MS/MS)测定气相空气中多环芳烃的方法。","authors":"Ping Wang, Zhong-Min Wang, Jeff Wagner, Kazukiyo Kumagai","doi":"10.1016/j.chroma.2025.465689","DOIUrl":null,"url":null,"abstract":"<div><div>A solvent-free, thermal extraction method for analysis of polycyclic aromatic hydrocarbons (PAHs) in gas phase airborne samples was developed. A fully automated thermal desorber (TD) coupled with highly selective and sensitive gas chromatography-tandem mass spectrometry (GC–MS/MS) was used to determine the concentration of trace level PAHs. Air sampling was conducted to tune the sampling and analytical conditions. Various instrument operating parameters such as sorbent tube desorption temperature/time, cold trap desorption temperature/time, outlet split ratio, tube storage stability, as well as air sampling flow rate and time were tested to optimize the analytical conditions. Method performance showed linearity in broad range (0.01 to 10 ng) with regression coefficients of external calibration curves (R<sup>2</sup>) >0.998 for all targeted PAHs. Method detection limit (MDL) was between 0.01–0.05 ng per tube. The method precision (<20 %) and accuracy were also satisfactory, obtaining quantitative recoveries (mean values between 80 and 120 %). The method has been applied for both outdoor and indoor air analysis. Small volume of air sample (<144 L) was sufficient for the PAH analysis. Naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, anthracene, fluoranthene, acenaphthene, fluorene, pyrene, and acenaphthylene are the primary PAHs in the gas phase for both indoor and outdoor air. Naphthalene and its two methylated compounds: 1-methylnaphthalene and 2-methylnaphthalene accounted for 47.7 % and 81.7 % of the total gas phase PAHs for outdoor and indoor, respectively. Using thermal extraction instead of organic solvent extraction for sample pretreatment makes the method sustainable and in consonance with the principles of green chemistry. No solvent and time-consuming extract step are needed. The method greatly improved the analytical process with a fully automated TD-GC–MS/MS instrument.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1744 ","pages":"Article 465689"},"PeriodicalIF":4.0000,"publicationDate":"2025-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"A solvent-free thermal desorption-gas chromatography-tandem mass spectrometry method (TD-GC–MS/MS) for the determination of polycyclic aromatic hydrocarbons in gas phase airborne samples\",\"authors\":\"Ping Wang, Zhong-Min Wang, Jeff Wagner, Kazukiyo Kumagai\",\"doi\":\"10.1016/j.chroma.2025.465689\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>A solvent-free, thermal extraction method for analysis of polycyclic aromatic hydrocarbons (PAHs) in gas phase airborne samples was developed. A fully automated thermal desorber (TD) coupled with highly selective and sensitive gas chromatography-tandem mass spectrometry (GC–MS/MS) was used to determine the concentration of trace level PAHs. Air sampling was conducted to tune the sampling and analytical conditions. Various instrument operating parameters such as sorbent tube desorption temperature/time, cold trap desorption temperature/time, outlet split ratio, tube storage stability, as well as air sampling flow rate and time were tested to optimize the analytical conditions. Method performance showed linearity in broad range (0.01 to 10 ng) with regression coefficients of external calibration curves (R<sup>2</sup>) >0.998 for all targeted PAHs. Method detection limit (MDL) was between 0.01–0.05 ng per tube. The method precision (<20 %) and accuracy were also satisfactory, obtaining quantitative recoveries (mean values between 80 and 120 %). The method has been applied for both outdoor and indoor air analysis. Small volume of air sample (<144 L) was sufficient for the PAH analysis. Naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, anthracene, fluoranthene, acenaphthene, fluorene, pyrene, and acenaphthylene are the primary PAHs in the gas phase for both indoor and outdoor air. Naphthalene and its two methylated compounds: 1-methylnaphthalene and 2-methylnaphthalene accounted for 47.7 % and 81.7 % of the total gas phase PAHs for outdoor and indoor, respectively. Using thermal extraction instead of organic solvent extraction for sample pretreatment makes the method sustainable and in consonance with the principles of green chemistry. No solvent and time-consuming extract step are needed. 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引用次数: 0
摘要
建立了一种分析气相空气样品中多环芳烃(PAHs)的无溶剂热萃取方法。采用全自动热脱附器(TD)结合高选择性、高灵敏度的气相色谱-串联质谱(GC-MS/MS)测定痕量多环芳烃的浓度。进行空气采样以调整采样和分析条件。测试了吸附管解吸温度/时间、冷阱解吸温度/时间、出口劈裂比、管储存稳定性、空气采样流量和时间等仪器运行参数,优化了分析条件。方法在0.01 ~ 10 ng范围内呈良好的线性关系,外标曲线回归系数(R2)均为>0.998。方法检测限(MDL)为0.01 ~ 0.05 ng /支。方法精度(
A solvent-free thermal desorption-gas chromatography-tandem mass spectrometry method (TD-GC–MS/MS) for the determination of polycyclic aromatic hydrocarbons in gas phase airborne samples
A solvent-free, thermal extraction method for analysis of polycyclic aromatic hydrocarbons (PAHs) in gas phase airborne samples was developed. A fully automated thermal desorber (TD) coupled with highly selective and sensitive gas chromatography-tandem mass spectrometry (GC–MS/MS) was used to determine the concentration of trace level PAHs. Air sampling was conducted to tune the sampling and analytical conditions. Various instrument operating parameters such as sorbent tube desorption temperature/time, cold trap desorption temperature/time, outlet split ratio, tube storage stability, as well as air sampling flow rate and time were tested to optimize the analytical conditions. Method performance showed linearity in broad range (0.01 to 10 ng) with regression coefficients of external calibration curves (R2) >0.998 for all targeted PAHs. Method detection limit (MDL) was between 0.01–0.05 ng per tube. The method precision (<20 %) and accuracy were also satisfactory, obtaining quantitative recoveries (mean values between 80 and 120 %). The method has been applied for both outdoor and indoor air analysis. Small volume of air sample (<144 L) was sufficient for the PAH analysis. Naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, anthracene, fluoranthene, acenaphthene, fluorene, pyrene, and acenaphthylene are the primary PAHs in the gas phase for both indoor and outdoor air. Naphthalene and its two methylated compounds: 1-methylnaphthalene and 2-methylnaphthalene accounted for 47.7 % and 81.7 % of the total gas phase PAHs for outdoor and indoor, respectively. Using thermal extraction instead of organic solvent extraction for sample pretreatment makes the method sustainable and in consonance with the principles of green chemistry. No solvent and time-consuming extract step are needed. The method greatly improved the analytical process with a fully automated TD-GC–MS/MS instrument.
期刊介绍:
The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.