摘要
建立溶剂解吸-气相色谱-质谱法测定空气中异亚丙基丙酮和乙基戊基甲酮两种脂肪酮。用活性炭管采集空气样品,以二硫化碳溶液解吸,采用气相色谱-质谱联用仪检测。选择分流模式进样,样品经DB-624毛细管色谱柱(30 m×0.32 mm,1.80μm)程序升温分离,利用多反应离子监测模式扫描,以保留时间和特征质量离子定性,外标法定量。异亚丙基丙酮和乙基戊基甲酮的质量浓度分别在0.02~200.0、0.01~100.0μg/mL范围内与定量离子的色谱峰面积线性关系良好,相关系数分别为0.998、0.999 1,方法检出限分别为0.02、0.01μg/mL,定量限分别为0.06、0.03μg/mL。样品加标平均回收率分别为93.6%~102%和98.1%~100%,测定结果的相对标准偏差分别为0.83%~3.6%和3.0%~5.2%(n=6)。样品在室温下可保存3 d, 4℃冷藏可保存7 d。该方法适用于空气中异亚丙基丙酮和乙基戊基甲酮的检测。
A method of solvent desorption-gas chromatography-mass spectrometry was established for the determination of ethyl amyl ketone and mesityl oxide in air.The samples were collected with activated carbon tubes,desorbed by carbon disulfide solution,and detected by gas chromatography-mass spectrometry.Samples were introduced in split flow mode,separated using a DB-624 capillary chromatography column(30 m×0.32 mm,1.80μm)with temperature programming,and analyzed via multiple reaction monitoring scanning.Analytes were identified by retention time and characteristic ions,and quantified by the external standard method.The mass concentrations of ethyl amyl ketone and mesityl oxide had good linear relationship with the chromatographic peak area of quantitative ions in the range of 0.02-200.0μg/mL and 0.01-100.0μg/mL,respectively,with correlation coefficients of 0.998 and 0.9991.The detection limits of the method were 0.02μg/mL and 0.01μg/mL,and the quantification limits were 0.06μg/mL and 0.03μg/mL,respectively.The average recoveries of samples spiked were 93.6%-102%and 98.1%-100%,and the relative standard deviations of determination results for six parallel samples were 0.83%-3.6%and 3.0%-5.2%,respectively.The samples remained stable for 3 days at room temperature and for 7 days when stored at 4℃.This method is applicable for the detection of ethyl amyl ketone and mesityl oxide in air.
作者
张来颖
宋文颉
李慧苗
刘裕婷
张志荣
王玉江
马晓曼
谢俊卿
ZHANG Laiying;SONG Wenjie;LI Huimiao;LIU Yuting;ZHANG Zhirong;WANG Yujiang;MA Xiaoman;XIE Junqing(Beijing Fengtai Center for Disease Control and Prevention,Beijing 100070,China)
出处
《化学分析计量》
2026年第1期111-118,共8页
Chemical Analysis And Meterage
关键词
脂肪酮
溶剂解吸
气相色谱-质谱法
空气
aliphatic ketone
solvent desorption
gas chromatography-mass spectrometry
air
