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使用Bond Elut Plexa固相萃取法和液相色谱-串联质谱法分析大米(水稻)中的溴硝醇(2-溴-2-硝基丙烷-1,3-二醇)残留量

Analysis of bronopol (2-bromo-2-nitropropan-1, 3-diol) residues in rice (Oryza sativa L.) by SPE using Bond Elut Plexa and liquid chromatography-tandem mass spectrometry.

作者信息

Chai Shuang-Shuang, Qin Mei-Ling, Ma You-Ning, Gao Huan-Huan, He Qiao, Zhang Han-Tong

机构信息

China National Rice Research Institute, No. 28, Rice Road, Zhejiang, Hangzhou, 310006, China.

出版信息

Anal Bioanal Chem. 2018 Jan;410(2):399-405. doi: 10.1007/s00216-017-0730-y. Epub 2017 Nov 21.

Abstract

A novel method has been developed for the direct, sensitive, and rapid detection of bronopol in rice using a simple solid-phase extraction (SPE) procedure followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), with electrospray ionization (ESI). Bronopol was stable under acidic conditions, and an acidic environment was thus needed before sample loading to ensure the stability of bronopol. Rice extracts containing bronopol were pretreated using a hydrophilic-lipophilic balanced (Bond Elut Plexa) cartridge to reduce the matrix effect. An XDB-C18 column (150 mm × 2.1 mm, 3.5 μm) was used for chromatographic separations, with a mobile phase comprising methanol and aqueous ammonium formate (5 mM). The linearity of the method was satisfactory with regression coefficient (R ) = 0.9992. The limit of quantification was 3.3 μg kg. Three spiked levels (25, 125 and 625 μg kg) were used to determine the recovery of bronopol, which was found to be 73.3-96.7%, with relative standard deviations (RSD) in the range 1.2-7.9%. The RSD for intra-day precision (n = 7) was 7.6% and the RSD for inter-day precision (n = 15) was 8.3%. The newly developed analytical method was successfully used to quantify bronopol in rice samples.

摘要

已开发出一种新颖的方法,用于直接、灵敏且快速地检测大米中的溴硝醇。该方法采用简单的固相萃取(SPE)程序,随后结合液相色谱 - 串联质谱(LC - MS/MS)及电喷雾电离(ESI)技术。溴硝醇在酸性条件下稳定,因此在进样前需要酸性环境以确保溴硝醇的稳定性。含有溴硝醇的大米提取物使用亲水亲脂平衡(Bond Elut Plexa)柱进行预处理,以降低基质效应。采用XDB - C18柱(150 mm×2.1 mm,3.5μm)进行色谱分离,流动相由甲醇和甲酸铵水溶液(5 mM)组成。该方法线性良好,回归系数(R)= 0.9992。定量限为3.3μg/kg。使用三个加标水平(25、125和625μg/kg)来测定溴硝醇的回收率,回收率为73.3 - 96.7%,相对标准偏差(RSD)在1.2 - 7.9%范围内。日内精密度(n = 7)的RSD为7.6%,日间精密度(n = 15)的RSD为8.3%。新开发的分析方法成功用于定量大米样品中的溴硝醇。

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