刘欣, 向海英, 张涛, 曾婉俐, 蒋次清, 王晋, 孔维松, 李晶. 水蒸气蒸馏分离-气相色谱/质谱法测定烟用香精和料液中的防腐剂*[J]. 云南大学学报(自然科学版), 2018, 40(3): 551-560. doi: 10.7540/j.ynu.20170557
引用本文: 刘欣, 向海英, 张涛, 曾婉俐, 蒋次清, 王晋, 孔维松, 李晶. 水蒸气蒸馏分离-气相色谱/质谱法测定烟用香精和料液中的防腐剂*[J]. 云南大学学报(自然科学版), 2018, 40(3): 551-560. doi: 10.7540/j.ynu.20170557
LIU Xin, XIANG Hai-ying, ZHANG Tao, ZENG Wan-li, JIANG Ci-qing, WANG Jin, KONG Wei-song, LI Jing. Steam distillation pretreatment coupled with GC-MS for determination of preservatives in flavouring and casing for tobacco[J]. Journal of Yunnan University: Natural Sciences Edition, 2018, 40(3): 551-560. DOI: 10.7540/j.ynu.20170557
Citation: LIU Xin, XIANG Hai-ying, ZHANG Tao, ZENG Wan-li, JIANG Ci-qing, WANG Jin, KONG Wei-song, LI Jing. Steam distillation pretreatment coupled with GC-MS for determination of preservatives in flavouring and casing for tobacco[J]. Journal of Yunnan University: Natural Sciences Edition, 2018, 40(3): 551-560. DOI: 10.7540/j.ynu.20170557

水蒸气蒸馏分离-气相色谱/质谱法测定烟用香精和料液中的防腐剂*

Steam distillation pretreatment coupled with GC-MS for determination of preservatives in flavouring and casing for tobacco

  • 摘要: 建立了水蒸气蒸馏分离-气相色谱/质谱法(GC-MS)测定烟用香精和料液中的防腐剂的方法.方法利用水蒸气蒸馏(110℃,5mL/min流量,收集22min,馏分90~95mL)进行目标物质分离,并利用Oasis HLB反相固相萃取柱进行溶剂转换及样品再净化,萃取柱利用5mL甲醇进行淋洗;滤液利用优化后的GC-MS法,选择离子模式进行检测;利用该方法,6种目标物质在0.2~120μg/mL范围内具有较好的线性(r>0.999),检出限在0.023~0.080μg/mL之间,定量限在0.070~0.25μg/mL之间,日间和日内精密度均小于5%,不同加标水平下,平均回收率在93%~103%之间.该方法广谱性强,灵敏度高,线性相关性好,重复性佳,可以满足烟用香料中防腐剂的检测及风险监控要求.

     

    Abstract: A method using steam distillation coupled with GC-MS was established to determine the content of the preservatives in flavouring and casing for tobacco.The steam distillation was operated under 110℃ at a steam flow-rate of 5mL/min for 22min and after the procedure about 90—95mL fraction was collected.Then the solid phase extraction(SPE) column was used for solvent conversion and further purification of the sample fraction with 5mL methanol as the eluent, and the eluent was tested by the optimized GC-MS with SIM detection mode.The target analytes could be separated smoothly with good linearity in the range of 0.2—120μg/mL with the correlation coefficients larger than 0.999.The limits of detection (LODs) were further evaluated (0.023—0.080μg/mL).The mean recovery of the target compounds at different spiked level was 93%—103% and the intra-day and inter-day precision were below 5%.With the advantages of applicability,high sensitivity and good reproducibility,this simple method was suitable for the monitoring analysis for preservatives and can be used for risk identification.

     

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