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固相萃取-加压毛细管电色谱法测定酵素中敌螨普的残留
引用本文:唐超,肖琦,付鹏.固相萃取-加压毛细管电色谱法测定酵素中敌螨普的残留[J].中国酿造,2022,41(10):226.
作者姓名:唐超  肖琦  付鹏
作者单位:(1.重庆安全技术职业学院 安全监督管理系,重庆 404020;2.重庆市万州食品药品检验所,重庆 404100)
摘    要:该研究建立了一种快速、高效的加压毛细管电色谱法检测酵素中敌螨普残留的分析方法,并依据所建立的方法研究不同酵素中敌螨普残留的情况。样品经体积分数20%的乙腈提取,PRiME HLB小柱净化后检测。以乙腈-15 mmol/L磷酸钾缓冲液(pH 4.7)(15∶85,V/V)为流动相,在电压强度+2 kV条件下,外标法峰面积定量。结果表明,敌螨普标准溶液在0.001~0.200 μg/mL质量浓度范围内线性良好,相关系数R为0.999 1,检出限(LOD)为1.0 μg/kg,定量限(LOQ)为3.0 μg/kg,加标回收率达到85.6%~92.9%,精密度试验结果相对标准偏差(RSD)为2.83%~5.12%。该方法具有前处理简单、快速的优点,适用于多种酵素中敌螨普残留分析。

关 键 词:固相萃取  加压毛细管电色谱法  酵素  敌螨普  农药残留  

Determination of dipteroparasin residue in Jiaosu by solid phase extraction-pressurized capillary electrochromatography
TANG Chao,XIAO Qi,FU Peng.Determination of dipteroparasin residue in Jiaosu by solid phase extraction-pressurized capillary electrochromatography[J].China Brewing,2022,41(10):226.
Authors:TANG Chao  XIAO Qi  FU Peng
Affiliation:(1.Department of Safety Supervision and Management, Chongqing Vocational Institute of Safety & Technology, Chongqing 404020, China; 2.Chongqing Wanzhou Food and Drug Inspection Institute, Chongqing 404100, China)
Abstract:In this study, a rapid and efficient method for the determination of dipteroparasin residues in Jiaosu by pressurized capillary electrochromatography was established, and the dipteroparasin residue in different Jiaosu was studied according to the established method. The samples were detected after extraction with 20% acetonitrile and purification with PRiME HLB column. Using acetonitrile-15 mmol/L potassium phosphate buffer (pH 4.7) (15∶85, V/V) as the mobile phase, and the peak area was quantified by external standard method under the condition of voltage intensity +2 kV. The results showed that the linearity of dipteroparasin standard solution was good in the mass concentration range of 0.001-0.200 μg/ml, the correlation coefficient R was 0.999 1, the limit of detection (LOD) was 1.0 μg/kg, the limit of quantification (LOQ) was 3.0 μg/kg, the recovery rate was 85.6%- 92.9%, and the relative standard deviation of precision tests results was 2.83%-5.12%. The method had the advantages of simple and rapid pretreatment, and was suitable for the analysis of dipteroparasin residues in a variety of Jiaosu.
Keywords:solid phase extraction  pressurized capillary electrochromatography  enzymes  dipteroparasin  pesticide residue  
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