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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
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2017-11-21 , DOI: 10.1007/s00216-017-0730-y
Shuang-shuang Chai , Mei-ling Qin , You-ning Ma , Huan-huan Gao , Qiao He , Han-tong Zhang

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 2) = 0.9992. The limit of quantification was 3.3 μg kg−1. Three spiked levels (25, 125 and 625 μg kg−1) 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.



中文翻译:

大米中溴硝酚(2-溴-2-硝基丙烷-1,3-二醇)残留量的分析(水稻 L.)通过Bond Elut Plexa和液相色谱-串联质谱法进行固相萃取

已开发出一种新颖的方法,可通过简单的固相萃取(SPE)程序,液相色谱-串联质谱(LC-MS / MS),电喷雾电离(直接电离)直接,灵敏和快速地检测大米中的溴硝酚( ESI)。Bronopol在酸性条件下是稳定的,因此在上样之前需要一个酸性环境以确保Bronopol的稳定性。使用亲水-亲脂平衡(Bond Elut Plexa)药筒对含有溴酚的大米提取物进行预处理,以降低基质效应。XDB-C18色谱柱(150 mm×2.1 mm,3.5μm)用于色谱分离,流动相包含甲醇和甲酸铵水溶液(5 mM)。该方法的线性与回归系数(R 2)= 0.9992。定量限为3.3μgkg -1。使用三个加标水平(25、125和625μgkg -1)测定溴硝的回收率,发现溴硝的回收率为73.3–96.7%,相对标准偏差(RSD)的范围为1.2–7.9%。日内精确度(n  = 7)的RSD为7.6%,日间精确度(n  = 15)的RSD为8.3%。新开发的分析方法已成功用于定量大米样品中的溴硝酚。

更新日期:2017-11-21
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