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投稿时间:2015-05-23
投稿时间:2015-05-23
中文摘要: 建立了分散固相萃取-高效液相色谱-串联质谱法测定椰汁中γ-壬内酯含量的方法,对提取条件、流动相、质谱条件进行了研究,并对γ-壬内酯可能的断裂机理进行了推测。待测样品直接用乙腈提取,PSA分散固相萃取,采用电喷雾离子源(ESI)、多反应监测正离子模式扫描,选择m/z 157.1/139.1、m/z 157.1/121.1作为γ-壬内酯的定性、定量离子对,外标法定量。γ-壬内酯在0.025μg/mL~0.50μg/mL范围内浓度与峰面积呈良好的线性关系,仪器检出限为0.025 μg/mL,方法的检测限为0.10mg/kg,定量限为0.40 mg/kg,添加水平为0.10、0.20、0.40 mg/kg时γ-壬内酯的平均回收率范围分别为92.4%~98.4%,相对标准偏差为6.8%~7.6%(n=10)。
中文关键词: γ-壬内酯 椰汁 分散固相萃取 高效液相色谱-串联质谱
Abstract:A dispersive solid phase extraction coupled with high performance liquid chromatography tandem mass spectrometry method with dispersive solid phase extraction was established for the determination of γnonanolactone in coconut juice.The effect of extration condition,flow phase,and tandem mass spectrometry parameters were investigated.And the possible fragmentation mechanisms of γ-nonanolactone were presumed.The sample was extracted with acetonitrile and determined under the multiple reaction monitoring(MRM)mode by employing external method.The precursor-product ion pair m/z 157.1/139.1 was selected as qualitative ions,and m/z 157.1/121.1 was selected as quantitaive ion.The calibration curve was linear in the range of 0.025 μg/mL~0.50 μg/mL.The limits of detection were 0.025 μg/mL for the instrument and 0.10 mg/kg for the method respec tively.The LOQ was 0.40 mg/kg for the method.The average recoveries of γ-nonanolactone were between 92.4%and 98.4%at spiked levels of 0.10,0.20 mg/kg and 0.40 mg/kg with relative standard derivation(RSDs)of 6.8%~7.6%(n=10).
keywords: γ-nonanolactone coconut juice dispersive solid-phase extraction high performance liquid chromatography tandem mass spectrometry
文章编号:201611026 中图分类号: 文献标志码:
基金项目:国家质检总局科技计划项目(2013IK153);海南省重点科技计划项目(ZDXM2014083);国家自然科学基金项目(31360447);海南省自然科学基金项目(212018;313105)
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