特丁基二甲基硅烷衍生化气相色谱-质谱联用法快速测定苹果汁中的棒曲霉素

Rapid determination of patulin in apple juice by tert-butyldimethylsilyl derivatization-gas chromatography-mass spectrometry

运用特丁基二甲基硅烷(TBDMS)衍生化气相色谱-质谱(GC-MS)联用法快速、高灵敏地测定了苹果汁中的棒曲霉素(PAT)。样品用乙酸乙酯-正己烷提取,Carb/C18混合型固相萃取柱净化,TBDMS衍生,GC-MS测定,选择离子监测(SIM)模式,外标法定量。在0.01～1mg/L的范围内线性良好(r>0.98),在2～50μg/kg的添加水平范围内,平均回收率为88%～98%,相对标准偏差(RSD)为5.3%～13.6%,PAT的检出限为0.5μg/kg,测定低限为2μg/kg。该方法快速、高灵敏、准确、专一、耐用,适合对苹果汁中PAT进行确证和定量测定。

A gas chromatography-mass spectrometry （GC-MS） method for the quantitative determination and confirmation of patulin in apple juice by tert-butyldimethylsilyl （TBDMS） derivatization was established.The sample was extracted with ethyl acetate-hexane and an aliquot of the supernatant was cleaned up using mixed-mode solid phase extraction （SPE） cartridge containing C18 and graphitized carbon black （GCB）,evaporated to dryness under nitrogen gas and the residue was converted to tert-butyldimethylsilyl derivative which was determined with GC-MS in selected ion monitoring （SIM） mode and external standard method was used for quantitative determination.The linear range was from 0.01 to 1 mg/L.The average recoveries were 88%-98% and relative standard deviations were 5.3%-13.6% in the spiked range of 2-50 μg/kg.The limit of detection was 0.5 μg/kg and the limit of quantification and confirmation was 2 μg/kg.The method is rapid,highly sensitive,accurate,specific,rugged and suitable for the quantitative determination and confirmation of patulin in apple juice.