食品科学

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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   

  1. 黑龙江出入境检验检疫局,黑龙江 哈尔滨 150001
  • 出版日期:2015-02-25 发布日期:2015-02-16
  • 基金资助:

    国家认证认可管理委员会资助项目(2009B548)

Determination of Ethylenediaminetetraacetic Acid Disodium Residues in Canned Eight-Ingredient Porridge by UPLC-MS-MS

YANG Changzhi, HAN Guangyuan, JIANG Bing, WEI Dongxu, CHENG Yang   

  1. Heilongjiang Entry and Exit Inspection and Quarantine Bureau, Harbin 150001, China
  • Online:2015-02-25 Published:2015-02-16

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 aciddisodium,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-串联质谱仪检测和确证,外标法定量。EDTA-2Na质量浓度在1.0~50.0 μg/mL范围内时,线性关系良好,EDTA-2Na的相关系数(R2)为0.992 2。在20~400 mg/kg添加范围内,样品平均加标回收率在79.4%~105.3%之间,相对标准偏差为7.93%~9.94%。EDTA-2Na的最低检出限为20 mg/kg。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

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) 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 external standard method. The linear range
was 1.0–50.0 μg/mL for EDTA-2Na with a correlation coefficient (R2) 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 mg/kg 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: ethylenediaminetetraacetic acid disodium (EDTA-2Na), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS), canned eight-ingredient porridge

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