摘要
目的建立适合于检测酸奶中微量苯及其同系物的顶空固相微萃取-气质联用检测方法。方法采用顶空固相微萃取进行目标物分离富集,用萃取头进行固相微萃取后上机测定,顶空固相微萃取条件为样品装液量10 mL,NaCl添加量2.0 g,转子设定转速为5000 r/min,萃取时间20 min,萃取温度60℃。采用相对校正因子内标法对苯系物进行定量分析。结果以氯苯为内标物,苯、甲苯、对（间）二甲苯、邻二甲苯、苯乙酮的相对校正因子依次为：10.87、3.07、0.34、0.55、4.867,检出限依次为：2、0.05、0.01、0.01、0.05μg/L（信噪比S/N≥3）,定量限依次为：5、0.12、0.05、0.06、0.15μg/L（信噪比S/N≥10）。苯系物的加标回收率为82%~104%,相对标准偏差（RSD）均小于4%。采用此方法对6种酸奶样品进行检测,苯系物的含量在4~24μg/L范围之间。结论该方法灵敏度高,准确性好,能够很好的检测酸奶中的苯系物含量。
Objective To establish a qualitative and quantitative method for the determination of BTEX（benzene,toluene,xylene,acetophenone） in yogurt by headspace solid-phase microextraction and gas chromatography mass spectrometry technology.Methods The headspace solid-phase microextraction conditions were as follows：sample volume 10 mL,amount of NaCl 2.0 g,extraction time 20 min,and extraction temperature 60 ℃.Relative correction factor was used for the quantitative analysis of BTEX.Results Chlorobenzene was used as the internal standard substance and the relative correction factors of benzene,toluene,p（m）-xylene,o-xylene and acetophenone were 10.87,3.07,0.34,0.55 and 4.867,respectively.The limits of detection（LODs） of benzene,toluene,p（m）-xylene,o-xylene and acetophenone were 2,0.05,0.01,0.01,0.05 μg/L（S/N≥3）,respectively,and the limits of quantification were 5,0.12,0.05,0.06,0.15 μg/L（S/N≥ 10）,respectively.The recoveries of BTEX were 82%~104%and RSD were less than 4%.The content of BTEX in 6 kinds of yogurt samples was in the range of 4~24 μg/L detected by this method.Conclusion The established method has excellent accuracy and sensitivity,which can be used to detect the trace BTEX in yogurt.
出处
《食品安全质量检测学报》
CAS
2016年第3期1123-1129,共7页
Journal of Food Safety and Quality
基金
国家"863"计划课题(2012AA101604)~~
关键词
酸奶
苯
苯同系物
气相色谱-质谱法
yogurt
benzene
benzologue
gas chromatography-mass spectrometry
