超声提取辅助顶空式固相微萃取/气相色谱-质谱法测定塑胶跑道面层中7种挥发性硫化物  

Detection of 7 Volatile Sulfur Compounds in Plastic Track Surface by Ultrasonic Extraction-HS-SPME/GC-MS Technique

作　　者：叶元坚 郑煜 蔡锦安 刘海燕 卢家俊 李晓增 陈伟力 YE Yuan-jian;ZHENG Yu;CAI Jin-an;LIU Hai-yan;LU Jia-jun;LI Xiao-zeng;CHEN Wei-li(Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447,China)

机构地区：[1]广州质量监督检测研究院,广东广州511447

出　　处：《分析测试学报》2022年第2期271-275,共5页Journal of Instrumental Analysis

基　　金：广州市市场监督管理局科技项目(2020kj02)。

摘　　要：建立了一种检测塑胶跑道面层中二甲基硫(DMS)、二硫化碳(CS2)、甲基乙基硫(MES)、二乙基硫(DES)、二甲基二硫(DMDS)、二乙基二硫(DEDS)、二甲基三硫(DMTS)7种挥发性硫化物(VSCs)的超声提取辅助顶空式固相微萃取/气相色谱-质谱(HS-SPME/GC-MS)分析方法。实验优化了顶空固相微萃取的萃取条件、超声提取条件及气相色谱-质谱参数。在优化条件下,DES、DMDS的线性范围为5~500 ng/g,其余5种VSCs的线性范围为10~500 ng/g,相关系数(r)为0.984 7~0.998 9,方法的检出限(S/N=3)为0.4~1.4 ng/g,定量下限(S/N=10)为1.3~4.7 ng/g。在低、中、高3个加标水平下的平均回收率为89.6%~104%,相对标准偏差(RSD,n=6)为3.5%~12%。该方法可实现分离、富集和进样一体化,适用于塑胶跑道面层中VSCs含量的日常检测。A gas chromatography-mass spectrometry(GC-MS)coupled with ultrasonic extraction and headspace solid phase microextraction(HS-SPME)was established for the rapid analysis of seven volatile sulfur compounds(VSCs),including dimethyl sulfide(DMS),carbon disulfide(CS2),methyl ethyl sulfide(MES),diethyl sulfide(DES),dimethyl disulfide(DMDS),diethyl disulfide(DEDS), dimethyl trisulfide(DMTS)in plastic track surface. The HS-SPME extraction conditions, ultrasonic extraction conditions and GC-MS parameters were optimized. Under the optimized conditions,7 VSCs had good linearities in the range of 5-500 ng/g for DES and DMDS,and10-500 ng/g for other five VSCs,with correlation coefficients(r)of 0. 984 7-0. 998 9.The limits of detection(LODs,S/N = 3)were in range of 0. 4-1. 4 ng/g,and the limits of quantitation(LOQs,S/N = 10)were 1. 3-4. 7 ng/g. The average recoveries at low, medium and high spiked levels ranged from 89. 6%to 104%,with relative standard deviations(RSDs,n = 6)of 3. 5%-12%.The method integrates separation,enrichment and injection into one step,and is suitable for the routine detection of VSCs in the synthetic surfaces.

关 键 词：顶空固相微萃取(HS-SPME) 气相色谱-质谱(GC-MS) 塑胶跑道面层 挥发性硫化物(VSCs) 

分 类 号：O657.3[理学—分析化学] O623.83[理学—化学]