IC-ICP-MS Determination of Residual Amounts of Bromate in Flour and Flour Products
摘 要
面粉样品用水分散,含油脂高的样品需另加石油醚,用超声提取和离心分离.分取一定量的上层清液流经On-Guard Ⅱ RP柱除去部分有机杂质,所得流出液用于离子色谱-电感耦合等离子体质谱法(IC-ICP-MS)测定其溴酸盐含量.为尽可能提高ICP-MS检测的灵敏度,选用了仪器高功率工作参数,质谱干扰主要是多原子干扰,选用同位素79Br作为测量同位素.由于经过了色谱柱分离,消除了多原子干扰,在离子色谱分析中采用硝酸及氨水作为流动相,溴酸盐工作曲线的线性范围为100 μg·L-1以内,方法的检出限(3σ/b)为0.6 μg·L-1.应用此方法分析了两种样品,测得平均回收率为97%,测定值的相对标准偏差(n=8)在3.3%~8.3%之间.
Abstract
Sample of flour or its products was dispersed with water (for fatty sample petroleum ether was added together with the water) and extracted ultrasonically.The mixture was centrifuged and a definite aliquot was taken for purification by passing through the On-Guard Ⅱ column to remove part of organic impuritres.Eluate from the column was used for IC-ICP-MS analysis to determined content of bromate.To achieve to the best sensitivity of the MS detection,high power parameters were adopted.The isotope 79Br was selected as the analytical isotope and the main MS interference of multi-atom was eliminated by separation on the chromatographic column.Nitric acid and aqueous ammonia were used as the mobile phase.Linearity range of the working curve was in the range within 100 μg·L-1 of BrO-3 ion.Detection limit (3σ/b) of the method found was 0.6 μg·L-1.The proposed method was used to analyze 2 kinds of samples for their bromate contents,giving value of average recovery of 97% and values of RSD′s (n=8) in the range of 3.3%-8.3%.
中图分类号 O657.63
所属栏目 工作简报
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收稿日期 2008/3/1
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备注杨振宇(1971-),男,上海市人,高级工程师,主要研究方向为食品理化分析.食品安全的整治工作.
引用该论文: YANG Zhen-yu,DENG Xiao-jun. IC-ICP-MS Determination of Residual Amounts of Bromate in Flour and Flour Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(4): 471~473
杨振宇,邓晓军. 离子色谱-电感耦合等离子体质谱法测定面粉及其制品中溴酸盐残留量[J]. 理化检验-化学分册, 2009, 45(4): 471~473
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参考文献
【1】王仲礼,赵晓红.溴酸钾及其替代物[J].面粉通讯,2006,2:36-38.
【2】SEUBERT A,SCHMINKE G,NOWAK M,et al.Comparison of on-line coupling of ion-chromatography with atmospheric pressure ionization mass spectrometry and with inductively coupled plasma mass spectrometry as tools for the ultra-trace analysis of bromate in surface water samples[J].J Chromatogr A,2000,884:191-199.
【3】MICHAEL N,ANDREAS S.Ultra-trace determination of bromate in drinking waters by means of microbore column ion chromatography and on-line coupling with inductively coupled plasma mass spectrometry[J].Anal Chim Acta,1998,359:193-204.
【4】王骏,张卉,祝建华.反相离子对液相色谱法测定小麦粉中的溴酸钾[J].食品科学,2007,28(1):270-272.
【5】GB/T 20188-2006小麦粉中溴酸盐的测定 离子色谱法[S].
【2】SEUBERT A,SCHMINKE G,NOWAK M,et al.Comparison of on-line coupling of ion-chromatography with atmospheric pressure ionization mass spectrometry and with inductively coupled plasma mass spectrometry as tools for the ultra-trace analysis of bromate in surface water samples[J].J Chromatogr A,2000,884:191-199.
【3】MICHAEL N,ANDREAS S.Ultra-trace determination of bromate in drinking waters by means of microbore column ion chromatography and on-line coupling with inductively coupled plasma mass spectrometry[J].Anal Chim Acta,1998,359:193-204.
【4】王骏,张卉,祝建华.反相离子对液相色谱法测定小麦粉中的溴酸钾[J].食品科学,2007,28(1):270-272.
【5】GB/T 20188-2006小麦粉中溴酸盐的测定 离子色谱法[S].
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