固相萃取-超高效液相色谱法测定土壤中氯吡苯脲的残留
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摘要
采用固相萃取-超高效液相色谱法(SPE-UPLC)快速测定土壤中的氯吡苯脲残留量,对比确定了合适的前处理方法,并系统优化了测定方法中的提取和净化条件。实验结果表明:当采用乙腈提取,超声时间为30 min,离心转速为5000 r/min,PSA柱净化,色谱流动相为:V乙睛∶V水=65∶35时土壤中氯吡苯脲的提取效果最佳。氯吡苯脲在0.05~5.0μg/m L质量浓度范围内与峰面积呈良好的线性关系(r=0.9999),定量限为0.025 mg/kg,氯吡苯脲的添加回收率为78.34%~102.4%,相对标准偏差为3.24%~6.65%。该方法测定速度快,准确度和精密度符合农药残留分析,能够满足对土壤中氯吡苯脲残留的快速测定要求。
The forchlorfenuron residues in soil were determined quickly by solid-phase extraction and ultra performance liquid chromatography( SPE-UPLC) in this paper. And this paper compared to determine the appropriate pre-treatment methods,optimized the extraction method and purification conditions.The optimal conditions were obtained that the sample was extracted with acetonitrile for 30 min by ultrasonic method, centrifuged in 5000 r/min and cleaned up with the PSA column.Forchlorfenuron was determined by ultra performance liquid chromatography using acetonitrile-water( 65 ∶ 35) as mobile phase.The developed method showed a good linear relationship in the range of 0.05 ~ 5.0 μg/m L for forchlorfenuron,with correlation coefficient of 0.9999.The limit of quantitation for forchlorfenuron was 0.025 mg/kg. The average recovery rates were78.34% ~102.4%,with relative standard deviation( RSD) ranging from 3.24% to 6.65%.The method is fast,highly sensitivity,repeatable and suitable for the determination of forchlorfenuron residues in soil.
The forchlorfenuron residues in soil were determined quickly by solid-phase extraction and ultra performance liquid chromatography( SPE-UPLC) in this paper. And this paper compared to determine the appropriate pre-treatment methods,optimized the extraction method and purification conditions.The optimal conditions were obtained that the sample was extracted with acetonitrile for 30 min by ultrasonic method, centrifuged in 5000 r/min and cleaned up with the PSA column.Forchlorfenuron was determined by ultra performance liquid chromatography using acetonitrile-water( 65 ∶ 35) as mobile phase.The developed method showed a good linear relationship in the range of 0.05 ~ 5.0 μg/m L for forchlorfenuron,with correlation coefficient of 0.9999.The limit of quantitation for forchlorfenuron was 0.025 mg/kg. The average recovery rates were78.34% ~102.4%,with relative standard deviation( RSD) ranging from 3.24% to 6.65%.The method is fast,highly sensitivity,repeatable and suitable for the determination of forchlorfenuron residues in soil.
引文
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[17]Shi X M,Jin F,Huang Y T,et al.Simultaneous determination of five plant growth regulators in fruits by modified quick,easy,cheap,effective,rugged,and safe(Qu ECh ERS)extraction and liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural&Food Chemistry,2015,60(1):60-65.
[18]李佳,龚道新.氯吡脲在土壤和黄瓜中的残留分析[J].湖南农业科学,2010(5):84-87.
[19]王慧君,薛亚薇,康健,等.SPE和Qu ECh ERS前处理方法结合LC-Q-TOF/MS检测苹果和番茄中282种农药残留对比研究[J].分析实验室,2015,34(4):383-387.
[20]吴杰,杨文友,王晓欢,等.固相萃取-超高效液相色谱法检测榨菜中氯吡苯脲的研究[J].食品工业科技,2017(3):286-289.
[21]孙大利,郑尊涛,叶火春,等.氯吡脲在葡萄中的残留分析方法及消解动态[J].农药,2011,50(10):751-753.
[22]吴莉莉,吕媛媛,沈兵,等.高效液相色谱-串联质谱法快速测定水果中氯吡脲残留量[J].理化检验-化学分册,2014,50(2):206-209.
[23]林涛,陈兴连,李彦刚,等.超高效液相色谱-串联质谱法测定葡萄中氯吡脲的残留[J].食品与机械,2013,29(6):93-98.
[24]侯玉茹,杨媛,石磊,等.固相萃取-高效液相色谱法检测葡萄中氯吡脲的研究[J].食品科技,2011,36(1):255-258.
[2]林利美,黄大伟,郭娇娇,等.氯吡脲对小鼠的毒性实验研究[J].食品工业科技,2012,33(14):360-362.
[3]张燕,舒平,徐幸,等.Florisil分散固相萃取-HPLC-MS/MS联用法测定果蔬中氯吡脲的残留[J].食品科学,2016,37(6):216-219.
[4]Chen W J,Jiao B N,Su X S,et al.Dissipation and residue of forchlorfenuron in citrus fruits[J].Bulletin of Environmental Contamination and Toxicology,2013,90(6):756-760.
[5]Liu Q,Gong D X,Peng X C,et al.Determination of forchlorfenuron dissipation and residue in cucumbers and red soil[J].Journal of Northeast Agricultural University(English Edition),2010,17(1):27-31.
[6]叶雪均,赵倩,郭子武,等.土壤微生物与有机农药互作关系及其应用[J].林业科技开发,2008,22(6):9-12.
[7]赵莉,马青,马琳,等.蔬菜瓜果中氯吡脲残留检测方法研究[D].武汉:华中农业大学,2007.
[8]张卫炜.氯吡脲的残留分析方法及残留动态研究[J].分析科学学报,2013,29(4):583-586.
[9]胡江涛,盛毅,方智,等.分散固相萃取_高效液相色谱法快速检测猕猴桃中的氯吡脲[J].色谱,2007,25(3):441-442.
[10]罗伟强,肖小华,杜卓,等.整体柱固相萃取-高效液相色谱法在线分析水果中的氯吡脲[J].色谱,2014(4):407-412.
[11]杨春平,李钊君,宁红,等.HPLC检测枇杷中氯吡脲含量的前处理方法[J].浙江大学学报(农业与生命科学版),2016,42(3):350-357.
[12]徐永,寿林飞,虞淼,等.超高效液相色谱-串联四级杆质谱联用法测定水果中多效唑、氯吡脲和咪鲜胺的残留[J].农药学学报,2012,14(1):61-66.
[13]Valverde A,Aguilera A,Ferrer C,et al.Analysis of forchlorfenuron in vegetables by LC/TOF-MS after extraction with the buffered Qu ECh ERS method[J].Journal of Agricultural&Food Chemistry,2010,58(5):2818-2823.
[14]白冰,赵莉,宋卫国,等.西瓜中氯吡脲残留的LC-MS/MS检测方法研究[J].上海农业学报,2016(3):60-62.
[15]Ma L Y,Zhang H Y,Xu W T,et al.Simultaneous determination of 15 plant growth regulators in bean sprout and tomato with liquid chromatography-triple quadrupole tandem mass spectrometry[J].Food Analytical Methods,2013,6(3):941-951.
[16]王楠,胡坪,国欣,等.Qu ECh ERS-HPLC法快速检测猕猴桃中氯吡脲残留[J].食品工业,2014(5):234-237.
[17]Shi X M,Jin F,Huang Y T,et al.Simultaneous determination of five plant growth regulators in fruits by modified quick,easy,cheap,effective,rugged,and safe(Qu ECh ERS)extraction and liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural&Food Chemistry,2015,60(1):60-65.
[18]李佳,龚道新.氯吡脲在土壤和黄瓜中的残留分析[J].湖南农业科学,2010(5):84-87.
[19]王慧君,薛亚薇,康健,等.SPE和Qu ECh ERS前处理方法结合LC-Q-TOF/MS检测苹果和番茄中282种农药残留对比研究[J].分析实验室,2015,34(4):383-387.
[20]吴杰,杨文友,王晓欢,等.固相萃取-超高效液相色谱法检测榨菜中氯吡苯脲的研究[J].食品工业科技,2017(3):286-289.
[21]孙大利,郑尊涛,叶火春,等.氯吡脲在葡萄中的残留分析方法及消解动态[J].农药,2011,50(10):751-753.
[22]吴莉莉,吕媛媛,沈兵,等.高效液相色谱-串联质谱法快速测定水果中氯吡脲残留量[J].理化检验-化学分册,2014,50(2):206-209.
[23]林涛,陈兴连,李彦刚,等.超高效液相色谱-串联质谱法测定葡萄中氯吡脲的残留[J].食品与机械,2013,29(6):93-98.
[24]侯玉茹,杨媛,石磊,等.固相萃取-高效液相色谱法检测葡萄中氯吡脲的研究[J].食品科技,2011,36(1):255-258.