A new solid-phase extraction and HPLC method for determination of patulin in apple products and hawthorn juice in China.
A new solid-phase extraction and HPLC method for determination of patulin in apple products and hawthorn juice in China.
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DOI：
10.1002/jssc.201100919
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发表时间：
2012-03
影响因子：
3.1
通讯作者：
Yuchun Zhou;W. Kong;Yan Li;A. Logrieco;Jun Xu;Meihua Yang
中科院分区：
文献类型：
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作者：
Yuchun Zhou;W. Kong;Yan Li;A. Logrieco;Jun Xu;Meihua Yang
采用自制的聚乙烯基聚吡咯烷酮-花色谱柱，建立了固相萃取前处理中国苹果、山楂产品中棒曲霉毒素的分析方法。用新方法制备了50个样品(苹果汁25个，苹果酱12个，山楂汁13个)，在Agela Venusil MP C(18)反相柱(4.6 mm×2 5 0 mm，5μm)上进行了高效液相色谱-二极管阵列检测。使用国产PVPP-F色谱柱对所有样品的净化结果与使用MycoSep®228 AflPat色谱柱的结果进行了比较。相关系数R(0.9998)在2.5~2 5 0μg/kg范围内与棒曲霉素线性关系良好。PVPP-F柱的检出限和定量限分别为3.99和9.64μg/kg，MycoSep®228Aflat柱的检出限和定量限分别为3.56和8.07μg/kg。样品中添加了25至250μg/kg的棒曲霉素，使用PVPP-F和MycoSep®228AflPAT色谱柱的回收率分别为81.9-100.9%和86.4-103.9%。在浓度为12.26~36.81μg/kg范围内，25份苹果汁样品中有2份(8.0%)和13份山楂汁样品中有1份(7.7%)含有自然产生的棒曲霉毒素。用LC-ESI-MS进一步证实了该方法的阳性结果。
A new solid-phase extraction (SPE) pretreatment method using a home-made polyvinylpolypyrrolidone-florisil (PVPP-F) column was developed for the analysis of patulin in apple and hawthorn products in China. Fifty samples (25 apple juices, 12 apple jams, and 13 hawthorn juices) were prepared using the new method and then analyzed by high performance liquid chromatography with diode array detection (HPLC-DAD) on an Agela Venusil MP C(18) reversed-phase column (4.6 mm × 250 mm, 5 μm). The cleanup results for all samples using home-made PVPP-F column were compared with those obtained using a MycoSep®228 AflaPat column. The correlation coefficient R (0.9998) fulfilled the requirement of linearity for patulin in the concentration range of 2.5-250 μg/kg. The limits of detection (LODs) and quantification (LOQs) of patulin were 3.99 and 9.64 μg/kg for PVPP-F column, and 3.56 and 8.07 μg/kg for MycoSep®228 AflaPat column, respectively. Samples were spiked with patulin at levels ranging from 25 to 250 μg/kg, and recoveries using PVPP-F and MycoSep®228 AflaPat columns were in the range of 81.9-100.9% and 86.4-103.9%, respectively. Naturally occurring patulin was found in 2 of 25 apple juice samples (8.0%) and 1 of 13 hawthorn juice samples (7.7%) at concentrations ranging from 12.26 to 36.81 μg/kg. The positive results were further confirmed by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS).