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

作　　者：刘欣 向海英 张涛 曾婉俐 蒋次清 王晋 孔维松 李晶 LIU Xin, XIANG Hai-ying, ZHANG Tao, ZENG Wan-li, JIANG Ci-qing, WANG Jin, KONG Wei-song, LI Jing(Technology Center, China Tobacco Yunnan Industrial Co., Lid, Kunming 650106, Chin)

机构地区：[1]云南中烟工业有限责任公司技术中心,云南昆明650106

出　　处：《云南大学学报（自然科学版）》2018年第3期551-560,共10页Journal of Yunnan University(Natural Sciences Edition)

基　　金：中国烟草总公司科技项目(110201502006);云南中烟工业有限责任公司资助项目(2016JC03)

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℃,5 m L/min流量,收集22 min,馏分90~95 m L)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5 m L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/m L范围内具有较好的线性(r>0.999),检出限在0.023~0.080μg/m L之间,定量限在0.070~0.25μg/m L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.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 5 m L/min for 22 min and after the procedure about 90—95 m L fraction was collected.Then the solid phase extraction（ SPE） column was used for solvent conversion and further purification of the sample fraction with 5 m L 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—120 μg/m L with the correlation coefficients larger than 0. 999. The limits of detection（ LODs） were further evaluated（ 0. 023—0.080 μg/m L）.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.

关 键 词：防腐剂 气相色谱质谱法(GC-MS) 水蒸气蒸馏 烟用香精 烟用料液 

分 类 号：TS426[农业科学—烟草工业]