磁性石墨烯固相萃取-液相色谱串联质谱法测定有机肥料中镇静剂类和β-受体激素类药物残留  

Determination of sedatives and β-receptor hormone drug residues in organic fertilizers by magnetic graphene solid phase extraction-liquid chromatography-tandem mass spectrometry

作　　者：王洪涛 许文娟 赵晗 崔晓娜 宫小明 刘文鹏 华萌萌 WANG Hong-tao;XU Wen-juan;ZHAO Han;CUI Xiao-na;GONG Xiao-ming;LIU Wen-peng;HUA Meng-meng(Weifang Customs of the People’s Republic of China,Weifang Shandong 261041;Shandong Animal Husbandry and Veterinary Vocational College,Weifang Shandong 261041)

机构地区：[1]中华人民共和国潍坊海关,山东潍坊261041 [2]山东畜牧兽医职业学院,山东潍坊261041

出　　处：《中国土壤与肥料》2022年第11期237-242,共6页Soil and Fertilizer Sciences in China

基　　金：济南海关科研项目(编号:2020JK004)。

摘　　要：采用磁性石墨烯固相萃取结合超高效液相色谱串联质谱技术,建立了有机肥料中8种镇静剂类和15种β-受体激素药物残留的分析检测方法。样品采用0.1%甲酸乙腈提取,通过磁性石墨烯粉固相萃取吸附目标物,除去杂质,然后再解吸目标物。经Agilent ZORBAX Eclipse Plus C18 (3.0 mm×100 mm,1.8μm)色谱柱分离,串联质谱进行检测,标准曲线内标法定量。结果表明:23种目标物在0.5~10.0μg/L范围内线性关系良好(R2>0.999)。在有机肥料样品基质中,目标化合物2、5、10μg/kg 3个加标水平的平均回收率在75.1%~102.4%之间,相对标准偏差为4.3%~14.3%(n=6)。该方法净化效率高、适用范围广,可用于有机肥料中镇静剂类和β-受体激素类药物残留筛查和检测。The analysis and detection method of 8 kinds of sedatives and 15 kinds of β-Receptor hormone drug residues in organic fertilizers were established by magnetic graphene solid phase extraction combined with liquid chromatography-tandem mass spectrometry.The sample was extracted with 0.1% formic acid acetonitrile.The target was adsorbed by magnetic graphene powder to remove impurities,and then the target was analyzed to obtain a clean sample matrix.Chromatographic column of Agilent ZORBAX Eclipse Plus C18(3.0 mm×100 mm,1.8 μm)was used for separation,liquid chromatographytandem mass spectrometry was adopted for detection,and standard curve internal standard method was used for quantification. The results showed that the linear of 23 targets was good in the range of 0.5 ~ 10.0 μg/L(R2>0.999).The average recoveries were 75.1%~102.4% in 2,5 and 10 μg/kg,and the relative standard deviation was 4.3%~14.3%(n=6).The method has high purification efficiency and wide application range,and can be used in the screening and detection of sedatives and β-receptor hormone drug residues in organic fertilizers.

关 键 词：高效液相色谱串联质谱 磁性石墨烯固相萃取 有机肥料 镇静剂类和β-受体激素 

分 类 号：TQ440.72[化学工程—化学肥料工业] O657.63[理学—分析化学]