UPLC-MS-MS法测定八宝粥罐头中乙二胺四乙酸二钠残留量.pdf

2082015,Vb.36,No.04
?品学
※安全检测
UPLC-MS-MS法测定八宝粥罐头中
乙二胺四乙酸二钠残留量
杨长志,韩广源,姜冰,魏冬旭,程阳
黑龙江出入境检验检疫局,黑龙江哈尔滨150001)
摘要;建立超高效液相色谱-串联质谱法测定八宝粥罐头中乙二胺四乙酸二钠( ethylenediaminetetraacetic acid
disodium,EDTA-2Na)残留量的检测和确证方法。试样中残留的EDTA-2Na用水高速匀浆提取,提取液经三氯
化铁衍生化、三氯甲烷和MAX阴离子交换柱净化后,用超高效液相色谱-申联质谱仪检测和确证,外标法定量。
EDTA-2Na质量浓度在1.0~50.0ug/mL范围内时,线性关系良好,EDTA-2Na的相关系数(R2)为0.9922。在
20~400mgkg添加范围内,样品平均加标回收率在79.4%~1053%之间,相对标准偏差为7.93%~9.94%。EDTA-2Na
的最低检出限为20mgkg。该方法具有灵敏、准确、稳定等优点,可用于八宝粥罐头中EDTA-2Na残留量测定。
关键词:乙二胺四乙酸二钠;超高效液相色谱-串联质谱;八宝粥罐头
Determination of Ethylenediaminetetraacetic Acid Disodium Residues in Canned Eight-ingredient
Porridge by UPLC-MS-MS
YANG Changzhi, HAN Guangyuan, JIANG Bing, WEI Dongxu, CHIENG Yang
(eilongjiang Entry and Exit Inspection and Quarantine Bureau, Harbin 150001, China)
Abstract: An ultra performance liquid chromaography-tandem mass pectrometry(oplc-ms-m)method was developed
for the determination and confirmation of ethylenediaminetetraacetic acid disodium(edta-2na)residues in canned
eight-ingredient porridge. The EDTA-2NA residues in the test samples were extracted with water by means of high-speed
homogenization. The extract was derivatized with Fecl3 reagent, cleaned up by chloroform and MAX anion exchange
column. The residues were determined and confirmed by UPLC-MS-MS using an extemal standard method. The linear rang
was 10-500 ug/ml for EDTA-2NA wih a comelation effcient(R)of 0.992 2. The average recoveries of EDTA-2NA in
spiked samples ranged from 79. 4%-105.3%, with relative standard deviations between 7.93% and 9.94% at spiked levels
of 20-400 mg/kg. The limit of detection was 20 mgkg for EDTA-2NA. The method is sensitive, accurate, repeatable and
suitable for the determination of EDTA-2NA residues in canned eight-ingredient porridge
Key words: ethylenediamineteraace ic acid disodium(edta-2na ultra performance liquid chromatography-tandem mass
spectrometry(uplc-ms-ms); canned eight-ingredient porridge
中图分类号:O657.6
文献标志码:A
文章编号:1002-6630(2015)04020805
doi:10.7506/spkx1002-6630-201504041
乙二胺四乙酸二钠( ethylenediaminetetraacetic acid0~-205mgkg。国外对EDTA在食品中的残留量有严格的
disodium,EDTA-2Na)是GB2760-2011《食品添加剂限量规定。日本规定罐头食品中EDTA的残留(以乙二
使用标准》允许使用的一种食品添加剂",可与铁、铜、胺四乙酸二钠钙计)不得超过250mg/kg,饮料中不得超
钙、镁等多价离子螯合成稳定的水溶性络合物,利用其过35mg/kg。我国在八宝粥等罐头食品中规定不得超过
络合作用来防止由金属引起的变色、变质、变浊及VC250mgkg
的氧化损失,起到护色、抗氧化作用。由于其良好的
目前,有关于食品中EDTA-2Na残留量国内报道很
添加效果,常被作为抗氧化剂、防腐剂、稳定剂和凝固多6,但针对八宝粥等罐头食品中EDTA-2Na残留检测
剂而广泛的应用于加工食品中明,但过多的EDTA-2Na被无文献报道,大多采用液相色谱法进行检测,样品经
人食入后,会对人身造成伤害,其每日允许摄入量值为
水提取,经CuC12或三氯化铁衍生后,采用离子对试剂
收稿日期:2014-03-18
基金项目:国家认证认可管理委员会资助项目(2009B548)
作者简介:杨长志(1962-),男,研究员,硕士,主要从事食品安全和检测研究。E-mail: yangtz621126@163.c0m
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