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同位素稀释-超高效液相色谱-串联质谱法检测蜂蜜中泛酸含量
引用本文:何敏恒,李秀英,曾令浩,黄景晟,郭新东.同位素稀释-超高效液相色谱-串联质谱法检测蜂蜜中泛酸含量[J].中国酿造,2015,34(4):157.
作者姓名:何敏恒  李秀英  曾令浩  黄景晟  郭新东
作者单位:广州质量监督检测研究院 国家加工食品质量监督检验中心(广州),广东广州511447
基金项目:国家质量监督检验检疫总局科技计划项目(2014QK052)
摘    要:建立了同位素稀释-超高效液相色谱-串联质谱法(UPLC-MS/MS)检测蜂蜜中泛酸(维生素B5)的快速定量和确证方法。样品经0.1%氨水(V/V)提取,MAX固相萃取柱净化后,以0.1%甲酸乙腈-0.1%甲酸水为流动相梯度洗脱,使用HSS T3色谱柱进行分离,电喷雾正离子多反应监测(MRM)模式检测,同位素内标法定量。在优化条件下,泛酸在0.500~500 μg/L范围内线性良好,相关系数(R2)为0.999 6;方法检出限为1.0 μg/kg(S/N=3),定量限为3.0 μg/kg(S/N=10);回收率在98.3%~98.7%之间,相对标准偏差(RSD)为2.4%~3.1%。通过市售蜂蜜样品测试表明,该方法操作简单、检测结果准确,可用于蜂蜜中泛酸的快速检测。

关 键 词:蜂蜜  泛酸  超高效液相色谱-串联质谱法  同位素稀释  

Determination of pantothenic acid in honey by isotope dilution-ultra performance liquid chromatography tandem mass spectrometry
HE Minheng,LI Xiuying,ZENG Linghao,HUANG Jingsheng,GUO Xindong.Determination of pantothenic acid in honey by isotope dilution-ultra performance liquid chromatography tandem mass spectrometry[J].China Brewing,2015,34(4):157.
Authors:HE Minheng  LI Xiuying  ZENG Linghao  HUANG Jingsheng  GUO Xindong
Affiliation:Guangzhou Quality Supervision and Testing Institute, National Centre for Quality Supervision and Testing of
Processed Food (Guangzhou), Guangzhou 511447, China
Abstract:A method for rapid quantification of pantothenic acid(PA) in honey by isotope dilution-ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed. The sample was extracted by 0.1% ammonia water (V/V), cleaned-up on Oasis MAX solid-phase extraction column, and finally separated by UPLC using a HSS T3 column, employing acetonitrile with 0.1% formic acid-0.1% formic as the mobile phase for gradient elution. The results were determined by tandem mass spectrometry with multiple reactions monitoring mode and quantified by internal standard method. The result indicated that the linear range was 0.500-500 μg/L, with the correlation coefficients of 0.999 6, the limits of detection (LOD, S/N=3) was 1.0 μg/kg, limits of quantification(LOQ, S/N=10) was 3.0 μg/kg, and the recovery rate ranged from 98.3% to 98.7% with RSD of 2.4%-3.1%(n=6). The sample testing results showed that the method was simple and accurate, and suitable for the determination of PA in honey.
Keywords:honey  pantothenic acid  UPLC-MS/MS  isotope dilution  
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