A method for the determination of chlorate and perchlorate in dried and fresh wolfberry by hot water bath extraction-dispersive solid phase extraction(DSPE)purification-ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The sample was ex-tracted by 7 ml ultra-pure water with water bath oscillations at 60℃ for 30 min,and then 13 ml methanol was added to vortex for 5 min.After centrifu-gation,the supernatants were purified by dispersed solid-phase extraction with C18 and graphitized carbon black(GCB).The purified liquid was deter-mined under electrospray negative ion source and multiple reaction monitoring(MRM)mode,and quantified by external standard method.The results showed that the linear relationship between chlorate and perchlorate in dried and fresh wolfberry was good within the range of 1.0-100.0 ng/ml and 0.5-100.0 ng/ml,respectively.The correlation coefficients R2 were 0.998 9 and 0.999 2,0.998 4 and 0.999 0,respectively.The limits of detection(LOD)and quantitation(LOQ)of chlorate were 1.0 μg/kg and 10.0 μg/kg,respectively,and the LOD and LOQ were 0.5 μg/kg and 5.0 µg/kg,re-spectively.The average adding standard recoveries of chlorate and perchlorate in dried and fresh wolfberry were 89.9％-93.4％and 76.8％-93.6％,re-spectively,with the relative standard deviations(RSD)lower than 11.0％and 12.0％,respectively.The average adding standard recoveries of chlorate and perchlorate were 73.8％-94.9％and 61.2％-90.5％,respectively,with RSD lower than 11.0％and 17.0％,respectively.
关键词
枸杞/氯酸盐/高氯酸盐/超高效液相色谱-串联质谱/热水浴提取/分散固相萃取净化
Key words
wolfberry/chlorate/perchlorate/UPLC-MS/MS/hot water bath extraction/dispersive solid phase extraction purification
维普
万方数据