水果中灭螨醌和羟基灭螨醌残留的高效液相色谱法测定  

Determination of acequinocyl and hydroxyacequinocyl in fruits by high-performance liquid chromatography

作　　者：陈波[1] 徐明敏[1] 金米聪[2,3] CHEN Bo XU Ming- min JIN Mi- cong(Beilun District Center for Disease Control and Prevention, Ningbo, Zhejiang 315800, China)

机构地区：[1]宁波市北仑区疾病预防控制中心,浙江宁波315800 [2]宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室,浙江宁波315010 [3]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010

出　　处：《中国卫生检验杂志》2017年第5期622-625,共4页Chinese Journal of Health Laboratory Technology

基　　金：宁波市科技创新团队项目(2015C110019);浙江省微量有毒化学物健康风险评估技术研究重点实验室开放基金(2014003)

摘　　要：目的建立水果中灭螨醌和羟基灭螨醌残留的固相萃取-高效液相色谱测定方法。方法水果样品经正己烷/乙酸乙酯(1∶1,V/V)溶液提取后,采用Cleanert Pesti Carb/NH_2固相萃取小柱净化,洗脱液经氮气流吹干后用0.1%(V/V)甲酸-乙腈(10∶90,V/V)溶液溶解。以Shim-pack XR-ODSⅡ柱(75 mm×2.0 mm,2.2μm)为分离柱、0.1%(V/V)甲酸-乙腈(10∶90,V/V)为流动相,等度洗脱,250 nm波长下进行紫外检测,外标法定量。结果灭螨醌和羟基灭螨醌在0.05 mg/L^5.0 mg/L具有良好的线性(r>0.999 0),检出限为0.002 mg/kg,定量限为0.007 mg/kg,回收率为84.5%~97.6%,相对标准偏差为1.7%~4.0%。结论本法具有简便、快速、准确的优点,可用于水果中灭螨醌和羟基灭螨醌的残留测定。Objective To develop a method for the simultaneous determination of acequinocyl and hydroxyacequinocyl in fruits by high-performance liquid chromatography（ HPLC） with solid-phase extraction.Methods The target compounds in fruit samples were successively extracted by n-hexane-ethyl acetate（ 1 ∶1,V/V）,cleaned up by using Cleanert Pesti Carb/NH2 cartridges,then evaporated to near dryness under a nitrogen stream,and finally dissolved in 0.1%（ V/V） formic acid/acetonitrile（ 10∶90,V/V）.Chromatographic separation was performed on a Shim-pack XR-ODS Ⅱ column（ 75 mm × 2.0 mm,2.2 μm） by using 0.1%（ V/V） formic acid/acetonitrile（ 10 ∶90,V/V） as the mobile phase in isocratic elution.Detection wavelenghth was 250 nm and quantification was based on external standard curves.Results Good linearities were obtained when the concentrations of acequinocyl and hydroxyacequinocyl were within 0.05 mg/L-5.0 mg/L,with correlation coefficients（ r） of 0.999 0.The detection limits of this method were 0.002 mg/kg,and the limits of quantification（ LOQs） were0.007 mg/kg for both acequinocyl and hydroxyacequinocyl.Recoveries were in the range of 84.5%-97.6%.The relative standard deviations（ RSDs） were within 1.7%-4.0%.Conclusion The developed method is simple,rapid and accurate,and it can be applied to the routine determination of acequinocyl and hydroxyacequinocyl in fruits.

关 键 词：高效液相色谱法 灭螨醌 羟基灭螨醌 水果 

分 类 号：O657.72[理学—分析化学]