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采用直接进样法建立并验证用于测定蜜露蜂蜜中酚类化合物的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)方法。

Development and validation of a LC-ESI-MS/MS method for the determination of phenolic compounds in honeydew honeys with the diluted-and-shoot approach.

作者信息

Seraglio Siluana Katia Tischer, Valese Andressa Camargo, Daguer Heitor, Bergamo Greici, Azevedo Mônia Stremel, Gonzaga Luciano Valdemiro, Fett Roseane, Costa Ana Carolina Oliveira

机构信息

Department of Food Science and Technology, Federal University of Santa Catarina, Florianopolis, SC, Brazil.

National Agricultural Laboratory (SLAV/SC/LANAGRO/RS), Ministry of Agriculture, Livestock and Food Supply, 88102-600, São José, SC, Brazil.

出版信息

Food Res Int. 2016 Sep;87:60-67. doi: 10.1016/j.foodres.2016.06.019. Epub 2016 Jun 22.

Abstract

A simple, reproducible and sensitive method has been optimized and validated for simultaneous determination of 32 phenolic compounds in bracatinga (Mimosa scabrella Benth.) with the diluted-and-shoot approach, without the need of any additional clean-up steps. It has been based on high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry and electrospray ionization (HPLC-ESI-MS/MS). The chromatography conditions were optimized, and due to the selectivity provided by MRM monitoring, LC separation required only 9min. The developed method was validated on the basis of Eurachem and European Commission Decision 2002/657/EC guidelines. Mean recoveries ranged from 70.4 to 110%. Intra-day and inter-day precision with RSD (relative standard deviations) from 0.14 to 18.9% and 0.34 to 20.0%, respectively were achieved. Limits of detection (LOD) and quantification (LOQ) ranged from 0.03 to 3.20μgL and 0.20-12.8μgL. Finally, the method was applied to samples and 20 phenolic compounds were quantified in all the samples analyzed, representing a contribution to the characterization and quantification of phenolic compounds from bracatinga (M. scabrella Bentham) honeydew honey.

摘要

已优化并验证了一种简单、可重复且灵敏的方法,采用稀释进样法同时测定巴西含羞草(Mimosa scabrella Benth.)中的32种酚类化合物,无需任何额外的净化步骤。该方法基于高效液相色谱-三重四极杆串联质谱联用和电喷雾电离(HPLC-ESI-MS/MS)。对色谱条件进行了优化,由于多反应监测(MRM)提供的选择性,液相色谱分离仅需9分钟。所开发的方法依据欧洲化学与分子光谱学学会(Eurachem)和欧盟委员会第2002/657/EC号决定的指导方针进行了验证。平均回收率在70.4%至110%之间。日内和日间精密度的相对标准偏差(RSD)分别为0.14%至18.9%和0.34%至20.0%。检测限(LOD)和定量限(LOQ)分别为0.03至3.20μg/L和0.20至12.8μg/L。最后,将该方法应用于样品分析,在所分析的所有样品中定量了20种酚类化合物,这为巴西含羞草(M. scabrella Bentham)蜜露蜂蜜中酚类化合物的表征和定量做出了贡献。

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