色谱 ›› 2017, Vol. 35 ›› Issue (8): 886-890.DOI: 10.3724/SP.J.1123.2017.04012

• 技术与应用 • 上一篇    下一篇

离子色谱-高分辨质谱法快速筛查乳制品中的酸度调节剂

云环1, 刘鑫1, 崔杰2, 杨婧1, 刘影2   

  1. 1. 北京出入境检验检疫局, 北京 100026;
    2. 北京工业技师学院, 北京 100023
  • 收稿日期:2017-04-11 出版日期:2017-08-08 发布日期:2013-11-25
  • 通讯作者: 刘鑫,Tel:58619861,E-mail:liuxin@bjciq.gov.cn
  • 基金资助:

    国家质检总局科研项目(2015IK013).

Rapid screening of acidity regulators in dairy by ion chromatography-high resolution mass spectrometry

YUN Huan1, LIU Xin1, CUI Jie2, YANG Jing1, LIU Ying2   

  1. 1. Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China;
    2. Beijing Industrial Technician College, Beijing 100023, China
  • Received:2017-04-11 Online:2017-08-08 Published:2013-11-25
  • Supported by:

    Science and Technology Planning Preject of General Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) (No. 2015IK013).

摘要:

建立了离子色谱-高分辨质谱(IC-HRMS)串联筛查乳制品中多种酸度调节剂的方法。乳制品样品用KOH溶液(pH调至7~8)提取,经Oasis MAX SPE柱净化,用Dionex IonPac AS11-HC柱(250 mm×4 mm)分离,Orbitrap检测器全扫描模式检测。以6种有机酸为例进行验证,在0.01~5.00 mg/L范围内线性相关系数均大于0.99。实际样品的加标回收率为74.3%~115.5%,相对标准偏差(RSD)为0.64%~4.81%(n=9)。将该法用于市售乳制品中酸度调节剂的筛查,在样品中可以筛查到苹果酸、柠檬酸、丁二酸、乳酸和己二酸。该方法快速、简便,可用于乳制品中多种酸度调节剂的定性筛查。

关键词: 快速筛查, 离子色谱-高分辨质谱, 乳制品, 酸度调节剂

Abstract:

A method for screening of acidity regulators in dairy based on ion chromatography-high resolution mass spectrometry technology (IC-HRMS) was set up. The dairy samples were extracted by KOH (pH 7-8) and Oasis MAX SPE column, and separated by a Dionex IonPac AS11-HC column (250 mm×4 mm). All the acidity regulators were detected by Orbitrap full scan mode. Taking six organic acids as an example, the calibration curves showed good linearities in the range of 0.05-5.00 mg/L, and the correlation coefficients (r) were higher than 0.99. By detecting the spiked samples, the recoveries were in the range of 74.3%-115.5% with the relative standard deviations (RSDs) between 0.64% and 4.81%. Malic acid, citric acid, lactic acid, succinic acid and adipic acid could be detected by IC-HRMS in the commercial dairy samples. The results indicate that the method is simple, rapid and suitable for the qualitative screening of acidity regulators in dairy products.

Key words: acidity regulators, dairy, ion chromatography-high resolution mass spectrometry (IC-HRMS), rapid screening

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