顶空固相微萃取-气相色谱-质谱法测定软木塞中愈创木酚的含量
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摘要
取磨碎的软木塞样品0.500 0g,用水超声提取30min,取提取液9mL置于萃取瓶中,加入1.8g Na2SO4,于55℃进行固相微萃取35min后,于气相色谱仪进样口解吸7min,采用气相色谱-质谱法测定其中愈创木酚的含量。结果表明:愈创木酚在25.00～2 000μg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.022μg·L-1,按标准加入法进行回收试验,回收率为69.8%～115%,测定值的相对标准偏差(n=6)为6.3%～13%。
The mashed cork sample(0.500 0 g)was extracted ultrasonically with water for 30 min,and 9 mL of the extract was taken and 1.8 g of Na2 SO4 were added into the extraction bottle.After solid-phase microextraction at 55℃for 35 min,the solution was desorbted for 7 min at the injection port of the gas chromatography,and guaiacol was determined by GC-MS.As shown by the results,linear relationship between values of peak area and mass concentration of guaiacol was found in the range of 25.00-2 000μg·L-1,with detection limit(3 S/N)of0.022μg·L-1.Test for recovery was made by standard addition method,giving results in the range of 69.8%-115%,and RSDs(n=6)ranged from 6.3%to 13%.
The mashed cork sample(0.500 0 g)was extracted ultrasonically with water for 30 min,and 9 mL of the extract was taken and 1.8 g of Na2 SO4 were added into the extraction bottle.After solid-phase microextraction at 55℃for 35 min,the solution was desorbted for 7 min at the injection port of the gas chromatography,and guaiacol was determined by GC-MS.As shown by the results,linear relationship between values of peak area and mass concentration of guaiacol was found in the range of 25.00-2 000μg·L-1,with detection limit(3 S/N)of0.022μg·L-1.Test for recovery was made by standard addition method,giving results in the range of 69.8%-115%,and RSDs(n=6)ranged from 6.3%to 13%.
引文
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[3]孙静,王锐,尹大强.顶空固相微萃取-气质联用法同时测定城市水源水中的九种嗅味物质[J].环境化学,2016,35(2):280-286.
[4]刘艳茹,梅勇,宋世震,等.顶空固相微萃取-气相色谱-质谱联用法测定土壤中甲基叔丁基醚[J].中国卫生检验杂志,2015,25(12):1913-1915.
[5]安代志,白淼,张灿,等.顶空固相微萃取-气相色谱/质谱联用分析果汁中愈创木酚和2,6-二溴苯酚[J].分析试验室,2016,35(4):440-442.
[2]ALVAREZ-RODRIGUEZ M L,BELLOCH C,VIL-LA M,et al.Degradation of vanillic acid and production of guaiacol by microorganisms isolated from cork samples[J].Fems Microbiology Letters,2003,220(1):49-55.
[3]孙静,王锐,尹大强.顶空固相微萃取-气质联用法同时测定城市水源水中的九种嗅味物质[J].环境化学,2016,35(2):280-286.
[4]刘艳茹,梅勇,宋世震,等.顶空固相微萃取-气相色谱-质谱联用法测定土壤中甲基叔丁基醚[J].中国卫生检验杂志,2015,25(12):1913-1915.
[5]安代志,白淼,张灿,等.顶空固相微萃取-气相色谱/质谱联用分析果汁中愈创木酚和2,6-二溴苯酚[J].分析试验室,2016,35(4):440-442.