气相色谱法测定茶叶中毒死蜱的样品前处理方法比较
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摘要
目的比较适用于茶叶中毒死蜱测定的样品前处理方法。方法茶叶经过研磨后准确称取5.00 g,加入30 ml丙酮或乙酸乙酯,涡旋混匀,通过超声、浸泡后超声、振荡3种方式提取,提取液于40℃旋转蒸发至近干;再将提取液用3 ml丙酮∶二氯甲烷(1∶1体积比)分3次溶解(1 ml×3)后通过Carb/NH2柱净化,净化液用氮气吹至近干;最后,使用丙酮定容至1 ml。Rtx-1701石英毛细管色谱柱分离,GC-FPD测定,外标法定量。结果超声、浸泡和振荡提取的回收率分别为87.4%~111.7%、84.6%~106.8%和88.5%~107.8%,相对标准偏差(RSD)分别为5.94%~7.00%、6.18%~6.73%和6.30%~6.98%。结论 3种不同提取方法的回收率均满足实验要求,超声提取省时,浸泡过夜后超声提取节省人力,振荡提取经典,但不适用于大批量样品,实际工作中可根据具体情况选择。
Objective To compare sample pretreatment methods about the determination of chlopyrifos in tea. Methods Tea samples were grounded and collected( 5. 00 g),adding 30 ml acetone or ethyl acetate to the samples,and then the samples were vortexmixed and extracted by ultrasound,soaking and ultrasound,and oscillation. The extract was rotarily evaporated to near dryness at 40 ℃,then dissolved in 3 ml of acetone: dichloromethane( 1∶1 by volume) for 3 times( 1 ml × 3) and then purified by a Carb/NH2 column and blown to nearly dry with nitrogen; finally,the residues were dissolved to constant volume 1 ml with acetone,and then separated with Rtx-1701 quartz capillary column,detected with GC-FPD,and external standard method was used for quantification. Results The recoveries of ultrasonic,soaking and oscillatory,oscillation were within87. 4%-111. 7%,84. 6%-106. 8% and 88. 5%-107. 8%,respectively. The relative standard deviations( RSDs) were within 5. 94%-7. 00%,6. 18%-6. 73% and 6. 30%-6. 98%,respectively. Conclusion The recovery rate of three different extraction methods all meet the requirement of experiment. Ultrasonic extraction saves time,soaking overnight after ultrasonic extraction save manpower,and oscillation extraction is classical,but not suitable for large quantities of samples. Actual work can be based on the specific circumstances of choice.
Objective To compare sample pretreatment methods about the determination of chlopyrifos in tea. Methods Tea samples were grounded and collected( 5. 00 g),adding 30 ml acetone or ethyl acetate to the samples,and then the samples were vortexmixed and extracted by ultrasound,soaking and ultrasound,and oscillation. The extract was rotarily evaporated to near dryness at 40 ℃,then dissolved in 3 ml of acetone: dichloromethane( 1∶1 by volume) for 3 times( 1 ml × 3) and then purified by a Carb/NH2 column and blown to nearly dry with nitrogen; finally,the residues were dissolved to constant volume 1 ml with acetone,and then separated with Rtx-1701 quartz capillary column,detected with GC-FPD,and external standard method was used for quantification. Results The recoveries of ultrasonic,soaking and oscillatory,oscillation were within87. 4%-111. 7%,84. 6%-106. 8% and 88. 5%-107. 8%,respectively. The relative standard deviations( RSDs) were within 5. 94%-7. 00%,6. 18%-6. 73% and 6. 30%-6. 98%,respectively. Conclusion The recovery rate of three different extraction methods all meet the requirement of experiment. Ultrasonic extraction saves time,soaking overnight after ultrasonic extraction save manpower,and oscillation extraction is classical,but not suitable for large quantities of samples. Actual work can be based on the specific circumstances of choice.
引文
[1]中华人民共和国卫生部.GB/T 5009.145—2003植物性食品中有机磷和氨基甲酸酯类农药多种残留的测定[S].北京:中国标准出版社,2003.
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[4]李伟,单美娜,徐晓枫,等.气相色谱法测定茶叶中3种有机氯和16种拟除虫菊酯农药残留[J].中国卫生检验杂志,2014,24(21):3062-3064.
[5]陈孝全,于星,吴晓刚,等.超声波辅助提取-气相色谱法测定茶叶中九种有机磷农药残留[J].湖北农业科学,2016,55(21):5623-5627.
[6]蒋定国,方从容,杨大进,等.测定茶叶中27中有机氯和拟除虫聚酯农药多组分残留气相色谱法[J].中国食品卫生杂志,2005,17(5):488-434.
[7]郭防.茶叶中农药残留检测的样品前处理研究进展[J].微量元素与健康研究,2012,29(1):61-64.
[8]杨大鹏.SPE柱净化-气相色谱法快速测定茶叶中的有机磷类农药残留量[J].中国卫生检验杂志,2014,24(20):3030-3031.
[9]蒋永祥,叶丽,汤淼荣.茶叶中7种有机磷农药残留量的同时测定[J].分析实验室2007,26(1):97-99.
[10]张有会,杨秀培,史兵方,等.气相色谱法测定蔬菜中有机磷农药残留的前处理方法比较[J].云南环境科学,2006,25(2):47-49.
[11]寇婷婷,徐昆龙,张灵芝,等.普洱茶中有机磷类农药残留的测定[J].食品科学,2010,31(12):165-168.
[12]卢剑,武中平,高巍,等.气相色谱双柱法测定茶叶中多种有机氯和拟除虫菊酯类农药残留量[J].食品科学,2009,30(24):401-404.
[13]林文华,罗慧明,蔡颖,等.气相色谱法测定蔬菜,水果中多种有机磷农药残留量[J].中国卫生检验杂志,2008,18(1):73-74.
[14]傅杭英.茶叶农药残留快速检测样品前处理技术研究[D].福建:福建农林大学,2013.
[15]蒋定国,杨大进,王竹天,等.茶叶中34种有机磷和氨基甲酸酯农药多残留的测定[J].中国卫生检验杂志,2007,17(3):157-159.
[2]中国标准化委员会.SN/T 1950—2007进出口茶叶中多种有机磷农药残留量的检验方法气相色谱法[S].北京:中国质检出版社,2014.
[3]杨大进,李宁.2014年国家食品污染和有害因素风险监测工作手册[M].北京:中国质检出版社,2014:126-129.
[4]李伟,单美娜,徐晓枫,等.气相色谱法测定茶叶中3种有机氯和16种拟除虫菊酯农药残留[J].中国卫生检验杂志,2014,24(21):3062-3064.
[5]陈孝全,于星,吴晓刚,等.超声波辅助提取-气相色谱法测定茶叶中九种有机磷农药残留[J].湖北农业科学,2016,55(21):5623-5627.
[6]蒋定国,方从容,杨大进,等.测定茶叶中27中有机氯和拟除虫聚酯农药多组分残留气相色谱法[J].中国食品卫生杂志,2005,17(5):488-434.
[7]郭防.茶叶中农药残留检测的样品前处理研究进展[J].微量元素与健康研究,2012,29(1):61-64.
[8]杨大鹏.SPE柱净化-气相色谱法快速测定茶叶中的有机磷类农药残留量[J].中国卫生检验杂志,2014,24(20):3030-3031.
[9]蒋永祥,叶丽,汤淼荣.茶叶中7种有机磷农药残留量的同时测定[J].分析实验室2007,26(1):97-99.
[10]张有会,杨秀培,史兵方,等.气相色谱法测定蔬菜中有机磷农药残留的前处理方法比较[J].云南环境科学,2006,25(2):47-49.
[11]寇婷婷,徐昆龙,张灵芝,等.普洱茶中有机磷类农药残留的测定[J].食品科学,2010,31(12):165-168.
[12]卢剑,武中平,高巍,等.气相色谱双柱法测定茶叶中多种有机氯和拟除虫菊酯类农药残留量[J].食品科学,2009,30(24):401-404.
[13]林文华,罗慧明,蔡颖,等.气相色谱法测定蔬菜,水果中多种有机磷农药残留量[J].中国卫生检验杂志,2008,18(1):73-74.
[14]傅杭英.茶叶农药残留快速检测样品前处理技术研究[D].福建:福建农林大学,2013.
[15]蒋定国,杨大进,王竹天,等.茶叶中34种有机磷和氨基甲酸酯农药多残留的测定[J].中国卫生检验杂志,2007,17(3):157-159.