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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 establish a solid-phase extraction and high performance liquid chromatographic method for the determination of quinacridone and hydroxyfenquone residues in fruits. Methods The fruit samples were extracted with hexane / ethyl acetate (1: 1, V / V) solution and cleaned up with Cleanert Pesti Carb / NH 2 solid phase extraction cartridges. The eluate was dried with nitrogen and then diluted with 0.1% / V) formic acid-acetonitrile (10:90, V / V) solution. The separation was performed on a Shim-pack XR-ODS II column (75 mm × 2.0 mm, 2.2 μm) with 0.1% (V / V) formic acid- UV detection at 250 nm wavelength, external standard method. Results The results showed that the linear range was 0.05 mg / L ~ 5.0 mg / L. The limit of detection was 0.002 mg / kg and the limit of quantification was 0.007 mg / kg. The recovery was 84.5% ~ 97.6%, the relative standard deviation was 1.7% ~ 4.0%. Conclusion This method is simple, rapid and accurate. It can be used to determine the residues of mite-quinone and hydroxy-mite quinone in fruits.