分散固相萃取结合超高效液相色谱-串联质谱法同时测定柑橘中春雷霉素与噻霉酮残留

建立了分散固相萃取结合超高效液相色谱-串联质谱(DSPE/UPLC-MS/MS)同时测定柑橘中春雷霉素和噻霉酮残留的分析方法。柑橘全果和果肉分别以含0.5%甲酸和含0.5%氨水的乙腈-水(7∶3,体积比)溶液提取,经十八烷基硅胶(C₁₈)净化上机,用Waters ACQUITY UPLC^? HSS T3色谱柱分离。以0.2%甲酸水-甲醇为流动相进行梯度洗脱,多反应离子监测模式(MRM)扫描,以基质匹配标准曲线外标法定量。结果显示:目标化合物在0.5～200μg/L质量浓度范围内线性关系良好(r²>0.999),检出限(LODs)为0.006～0.04μg/kg,定量下限(LOQs)为5～10μg/kg;加标回收率为73.4%～104%,相对标准偏差(RSD,n=6)为1.6%～9.6%。该方法易于操作,灵敏度高,适用于柑橘中春雷霉素和噻霉酮残留的同时检测。

Experimental Techniques and MethodsSimultaneous Determination of Kasugamycin and Benziothiazolinone Residues in Citrus by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

An analytical method was developed for the simultaneous determination of kasugamycin and benziothiazolinone residues in citrus by dispersive solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry(DSPE/UPLC-MS/MS).Citrus whole fruit and pulp were extracted with acetonitrile containing 0.5% formic acid and 0.5% aqueous ammonia-water(7 ∶3,by volume),respectively,then purified with octadecyl silica gel(C18) and separated on a Waters ACQUITY UPLC? HSS T3 column by gradient elution with 0.2% aqueous formic acid-methanol as mobile phase,finally analyzed in multiple reaction monitoring(MRM) mode and quantified by matrix-matched standard curve external standard method.Results showed that there were good linear relationships for the target compounds in the range of 0.5-200 μg/L with their correlation coefficients(r2) larger than 0.999.The limits of detection(LODs) and the limits of quantitation(LOQs) were in the concentration ranges of 0.006-0.04 μg/kg and 5-10 μg/kg,respectively.The spiked recoveries ranged from 73.4% to 104% with relative standard deviations(RSDs,n=6) of 1.6%-9.6%.With easy operation and high sensitivity,the method is suitable for the simultaneous determination of kasugamycin and benziothiazolinone residues in citrus.