HPLCMS/MS Determination of Na2EDTA in Food
摘 要
应用高效液相色谱串联质谱法(HPLCMS/MS)测定了食品中EDTA二钠盐。液态食品(5 g)直接加水40 mL提取;固态或酱状食品(5 g)加水15 mL及三氯甲烷20 mL匀质后离心,取其上清液,残渣重复提取2次。合并上清液,在提取液中加入三氯化铁溶液超声10 min衍生化后,定容至50 mL。取样品溶液5 mL,经MAX阴离子交换柱净化,用甲酸甲醇水(10+50+40)混合液6 mL洗脱,洗脱液经80 ℃吹氮蒸干,用水溶解后进行HPLCMS/MS分析。EDTA二钠盐的质量浓度在1.0~50.0 mg·L-1范围内呈线性。方法的检出限(3S/N)为5 mg·kg-1。应用提出的方法分析了4种食品样品并进行加标回收试验,测得回收率在88.3%~96.0%之间,测定值的相对标准偏差(n=6)均小于10%。
Abstract
HPLCMS/MS was applied to the determination of Na2EDTA in food. Na2EDTA in liquid samples (5 g) was extracted directly with 40 mL of water; while in solid or jam samples, was extracted by mixing and centrifuging with 15 mL of H2O and 20 mL of CHCl3, the supernatant was collected, and the lower phase was reextracted twice, the supernatants were collected and combined. The combined extract was then derivatized with FeCl3 solution by mixing ultrasonically for 10 min, and the mixture was made up to 50 mL. An aliquot of 5 mL of the derivatized solution was taken and purified by passing through MAX SPE column. The column was eluted with 6 mL of a mixture of HCOOHCH3OHH2O (10+50+40). The eluate was evaporated to dryness by N2blowing at 80 ℃, and the residue was dissolved with water. This solution was used for HPLCMS/MS analysis. Linearity range was found between 1.0-50.0 mg·L-1 for Na2EDTA. Detection limit (3S/N) found was 5 mg·kg-1. Four samples were analyzed by this method and test for recovery was made by standard addition method. Values of recovery obtained were in the range of 88.3%-96.0%, with RSD′s (n=6) all less than 10%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 哈尔滨市青年科技创新人才项目(2013RFQQJ175)
收稿日期 2013/5/16
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备注魏冬旭(1983-),女,河北昌黎人,工程师,硕士,主要从事食品安全检测。
引用该论文: WEI Dongxu,HAN Guangyuan,SUN Ying,HU Shaoxin,YANG Changzhi. HPLCMS/MS Determination of Na2EDTA in Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(6): 698~701
魏冬旭,韩广源,孙莹,胡少新,杨长志. 高效液相色谱-串联质谱法测定食品中的乙二胺四乙酸二钠[J]. 理化检验-化学分册, 2014, 50(6): 698~701
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参考文献
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【2】许中敏,鲍小丹,刘鲁林,等.乙二胺四乙酸铁钠(NaFeEDTA)的国内外法规情况研究[J].中国食品添加剂, 2012(1):207-211.
【3】吕晓华,文红,许红琴.高效液相色谱法测定板栗罐头中乙二胺四乙酸二钠的含量[J].中国卫生检验杂志, 2009,19(3):517-518.
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【9】李琛,李迎丽,唐开红.离子色谱法测定罐头、酱菜等食品中的EDTA2Na含量[J].中国卫生检验杂志, 2005,15(10):1233-1234.
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【14】姜华,蒙延峰,郑传波,等.Cu(Ⅱ)和Fe(Ⅲ)EDTA螯合物的反相离子对高效液相色谱分离和测定[J].烟台师范学院学报, 2005,21(4):275-278.
【15】SN/T 0001-1995出口商品中农药、兽药残留量及生物毒素检验方法标准编写的基本规定[S].
【2】许中敏,鲍小丹,刘鲁林,等.乙二胺四乙酸铁钠(NaFeEDTA)的国内外法规情况研究[J].中国食品添加剂, 2012(1):207-211.
【3】吕晓华,文红,许红琴.高效液相色谱法测定板栗罐头中乙二胺四乙酸二钠的含量[J].中国卫生检验杂志, 2009,19(3):517-518.
【4】施旭霞,陈笑梅.反相高效液相色谱法测定罐头食品中乙二胺四乙酸的残留量[J].色谱, 2000,18(5):445-447.
【5】郑睿行,张旭,方芳,等.高效液相色谱法测定酱腌菜制品中EDTA残留量[J].中国食品添加剂, 2011(2):156-159.
【6】罗祎,赵永彪,李淑娟,等.反相高效液相色谱法测定食品中EDTA的含量[J].中国食品添加剂, 2006(4):212-219.
【7】王琼,方艳红,徐金瑞.罐头食品中EDTA残留量的薄层色谱测定[J].华侨大学学报, 2002,23(1):37-39.
【8】CONGMIN Z X, TERRY H, PETER R, et al. EDTA in dairy wastewater and removal efficiencyA case study[J]. Civil and Envionmental Engineering, 2010,2(1):44-48.
【9】李琛,李迎丽,唐开红.离子色谱法测定罐头、酱菜等食品中的EDTA2Na含量[J].中国卫生检验杂志, 2005,15(10):1233-1234.
【10】QUINTANA J B, REEMTSMA T. Rapid and sensitive determination of ethylenediaminetetraacetic acid and diethylenetriaminepentaacetic acid in water samples by ionpair reversedphase liquid chromatographyelectrospray tandem mass spectrometry[J]. Chromatography A, 2007,1145:110-117.
【11】FINGERHUT R, DAME T, OLGEMOLLER B. Determination of EDTA in dried blood samplesby tandem mass spectrometry avoids serious errors in newborn screening[J]. Eur J Pediatr, 2009,168:553-558.
【12】SN/T 1018-2001出口食品罐头中乙二胺四乙酸含量检验方法[S].
【13】GB/T 21234-2007铁强化酱油中乙二胺四乙酸铁钠的测定[S].
【14】姜华,蒙延峰,郑传波,等.Cu(Ⅱ)和Fe(Ⅲ)EDTA螯合物的反相离子对高效液相色谱分离和测定[J].烟台师范学院学报, 2005,21(4):275-278.
【15】SN/T 0001-1995出口商品中农药、兽药残留量及生物毒素检验方法标准编写的基本规定[S].
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