建立了低温分配固液萃取(SLE-LTP)技术结合高效液相色谱-质谱(HPLC-MS)测定食用菌中6-苄基腺嘌呤(6-BA)的方法.食用菌样品经乙腈提取和低温分配,采用 Hitachi LaChrom C18色谱柱(250 mm×4.6 mm,5 μm)分离,以0.02 mol/L乙酸铵(含0.1%(v/v)冰乙酸)-甲醇(6:4,v/v)溶液为流动相,等度洗脱,在电喷雾正离子模式下检测,外标法定量.结果表明,6-苄基腺嘌呤在0.05~2.0 mg/L范围内线性关系良好,相关系数为1.0000;方法的检出限和定量限分别为0.006 mg/kg和0.02 mg/kg.加标回收率试验显示在0.1 mg/kg和0.5 mg/kg添加水平下6-苄基腺嘌呤的加标回收率为81.3%~93.7%,相对标准偏差为0.7%~2.4%.该法简单、准确、稳定,可用于食用菌中6-苄基腺嘌呤的检测.%A simple method based on solid liquid extraction with low-temperature partition (SLE-LTP)coupled with high performance liquid chromatography-mass spectrometry(HPLC-MS)was developed for the determination of 6-benzylaminopurine(6-BA)in edible mushrooms. The samples were extracted with acetonitrile followed by low-temperature partition at -30 ℃ for 4 h. The separation was performed on a Hitachi LaChrom C18 column(250 mm×4.6 mm,5 μm)with 0.02 mol/L ammonium acetate(containing 0.1%(v/v)glacial acetic acid)-methanol (6:4,v/v)as the mobile phases with isocratic elution. The compound was detected in positive electrospray ionization mode,and quantified by external standard method. The results showed that the limit of detection(LOD,S/N>3)for the analyte was 0.006 mg/kg,and the limit of quantification(LOQ,S/N>10)was 0.02 mg/kg. The calibration curve showed good linear in the range of 0.05-2.0 mg/L,and the correlation coefficient(r2)was 1.000 0. The spiked recoveries were between 81.3% and 93.7% with the relative standard deviations(RSDs,n=6) of 0.7%-2.4% at the spiked levels of 0.1 mg/kg and 0.5 mg/kg. The developed method is simple,reliable and can be applied for the accurate determination of 6-BA residue in edible mushrooms.
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