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 |
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基金项目:广州市市场监督管理局科技项目(2020kj02) |
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中文摘要: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。 |
中文关键词: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) |
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Detection of 7 Volatile Sulfur Compounds in Plastic Track Surface by Ultrasonic Extraction-HS-SPME/GC-MS Technique |
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Abstract: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,and 10-500 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. |
Key Words:headspace solid phase microextraction(HS-SPME) gas chromatography-mass spectrometry(GC-MS) plastic track surface volatile sulfur compounds(VSCs) |
引用本文:叶元坚,郑煜,蔡锦安,刘海燕,卢家俊,李晓增,陈伟力.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[J].分析测试学报,2022,41(2):271-275. |
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