超高效液相色谱串联质谱法测定果汁中的展青霉素.pdfVIP

2012年9月 Vol.30 No.9 September2012 ChineseJournal of Chromatography 957 ~961 技术与应用 DOI:10.3724/ SP.J.1123.2012.04026 超高效液相色谱-串联质谱法测定果汁中的展青霉素 ∗ 牛　 华,　 冯　 雷 ,　 牛之瑞,　 珠　 娜,　 祝红昆,　 王亚琴 (云南省产品质量监督检验研究院,云南 昆明650223) 摘要:建立了超高效液相色谱-电喷雾串联三重四极杆质谱(UPLC-ESI-MS/ MS)联用技术分析果汁中展青霉素的 方法。 浓缩果汁样品经酶解,乙酸乙酯提取,Oasis HLB 固相萃取(SPE)小柱净化后(澄清果汁直接进行 SPE净 化),以C18色谱柱为分离柱,以水和乙腈作为流动相进行梯度洗脱,电喷雾离子源电离、负离子多反应监测模式质 谱进行定性和定量分析。 展青霉素在1．0~500．0 μg/ L质量浓度范围内线性关系良好,相关系数为0．999,方法的 定量限为5．0 μg/ kg;加标水平为5．0、25．0 和 100．0 μg/ kg 时,加标回收率为80．6% ~91．8%,相对标准偏差为 1．5% ~7．3%。实验结果表明,该方法简单、灵敏、准确,各项技术指标均满足国内外法规要求,可用于果汁中展青霉 素的检测。 关键词:超高效液相色谱-串联质谱;固相萃取;展青霉素;果汁 中图分类号:O658　 　 　 文献标识码:A　 　 　 文章编号:1000-8713(2012)09-0957-05 Determination of patulin injuice by ultra performance liquid chromatography-tandem mass spectrometry ∗ NIU Hua,FENG Lei ,NIU Zhirui,ZHU Na,ZHU Hongkun,WANGYaqin (Yunnan Institute of Product QualitySupervision andInspection,Kunming 650223,China) Abstract:A method was developed for the simultaneous determination of patulin in juice by solid phase extraction (SPE)-ultra performance liquid chromatography coupled with electro- spray ionization tandem mass spectrometry (UPLC-ESI-MS/ MS). The cloudyjuice was hydro- lyzedby enzyme and extractedby ethyl acetate. The extract of cloudyjuicewas then enriched andpurifiedby an HLB SPE cartridge. If thejuice was clear it was directly treatedby the car- tridge as above.The separation was performed on a C18 column with the gradient elution of acetonitrile and water. The patulin was detected by MS with electrospray negative