摘要
建立了一种同时检测烟用水基胶中23种酯类化合物的液液萃取-气相色谱-质谱联用方法。23种酯类化合物包括乙酸酯类、丙烯酸酯类、甲基丙烯酸酯类、邻苯二甲酸酯类化合物。水基胶样品经水分散后，用含内标物丙酸珠乙酯的正已烷溶液振荡萃取，萃取液离心后过0．45μm有机相滤膜，用DB-WAXETR气相色谱柱（60m×0．25mm×0．25μm）分离，质谱选择离子模式监测，内标法定量。结果表明，23种酯类化合物在0．4—50．0mg／L范围内线性关系良好，线性相关系数大于0．998，样品加标回收率为81．8％～109．1％，相对标准偏差（RSD，n=5）小于4％，检出限为0．02～0．76mg／kg，定最限为0．04～2．52mg／kg。该方法前处理简便、快速、分析时间短、灵敏度高、重复性好，可用于烟用水基胶中23种酯类化合物的同时检测。
A method of gas chromatography-mass spectrometry （GC-MS） with liquid-liquid extraction has been developed for the simultaneous determination of 23 ester compounds inclu- ding acetate esters, acrylic esters, metacrylic acid esters and phthalate acid esters in cigarette water-borne adhesives. After dispersed in water, the sample was extracted by n-hexane solution containing phenyl ethyl propionate as internal standard substance. Then, the solution was centrifuged and filtrated through a 0.45 μm organic membrane filter. Finally, the solution was separated on a DB-WAXETR column （60 m ×0.25 mm ×0.25 μm）, and detected with MS in selected ion monitoring mode, and quantified by internal standard method. The results showed a good linear correlation in the range of 0.4 - 50.0 mg/L. The recoveries of the ester compounds spiked in the sample were 81.8% - 109. 1%, and the relative standard deviations （RSDs, = 5 ） were less than 4%. The limits of detection （LODs） and limits of quantification （LOQs） were in the ranges of 0.02 - 0.75 mg/kg and 0.04 - 2.52 mg/kg, respectively. The method is simple, time-saving, and has high sensitivity and good reproducibility. It can be applied to the determination of the 23 ester compounds in cigarette water-borne adhesives.
出处
《色谱》
CAS
CSCD
北大核心
2013年第10期989-994,共6页
Chinese Journal of Chromatography
基金
湖南中烟工业有限责任公司基金项目(2012-JC-0004)
关键词
液液萃取
气相色谱-质谱联用法
酯类化合物
烟用水基胶
liquid-liquid extraction
gas chromatography-mass spectrometry （GC-MS）
ester compounds
cigarette water-borne adhesives
