张 博,张 贺,刘思洁.分散微固相萃取-同位素内标法-超高效液相色谱-串联质谱法测定水果中的吗啉[J].食品安全质量检测学报,2018,9(4):918-924 |
分散微固相萃取-同位素内标法-超高效液相色谱-串联质谱法测定水果中的吗啉 |
Determination of morpholine in fruits by dispersive micro solid phase extraction-isotope internal standard-ultra performance liquid chromatography tandem mass spectrometry |
投稿时间:2017-11-21 修订日期:2018-02-01 |
DOI: |
中文关键词: 超高效液相色谱-串联质谱法 同位素内标法 分散微固相萃取 吗啉 水果 |
英文关键词:ultra performance liquid chromatography tandem mass spectrometry isotope internal standard method dispersive micro solid phase extraction morpholine fruits |
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中文摘要: |
目的 建立分散微固相萃取-同位素内标法-超高效液相色谱-串联质谱测定水果中吗啉残留量的检测方法。方法 样品经含1%甲酸的乙腈提取, 经分散微固相萃取净化、超高效液相色谱BEH HILIC色谱柱分离后, 经串联质谱检测, 同位素内标法定量。结果 吗啉在0~200 μg/L浓度范围内线性关系良好, 线性相关系数为0.9998。相对标准偏差(relative standard derivation, RSD)为1.2%~2.9%, 加标回收率为93.0%~101.6%。 结论 本方法采用同位素内标法, 具有灵敏度高、精密度和准确度好等优点, 简便快捷, 适合水果中吗啉的日常检测工作。 |
英文摘要: |
Objective To establish a method for determination of morpholine in fruits by dispersive micro solid phase extraction-isotope internal standard-ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS). Methods Samples were extracted by acetonitrile containing 1% formic acid, and purified by dispersive micro solid phase extraction (DMSPE). The analyte was separated on a BEH HILIC column, detected by mass spectrometry and quantified by isotope internal standard method. Results It showed good linear relationship in range of 0~200 μg/L for morpholine (r=0.9998). The relative standard derivations were 1.2%~2.9%, and the recoveries were 93.0%~101.6%. Conclusion This method use isotope internal standard method, and it is rapid, sensitive, and selective with excellent precision and accuracy, which can be used for daily detection of morpholine in fruits. |
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