色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 363-370.DOI: 10.3724/SP.J.1123.2014.12009

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定可食性包装材料中22种酸性染料

粟有志1, 刘俊2, 李芳1, 雷红琴1, 李艳美1, 刘绪斌1   

  1. 1. 伊犁出入境检验检疫局综合技术服务中心, 新疆 伊宁 835000;
    2. 新疆出入境检验检疫局技术中心, 新疆 乌鲁木齐 830063
  • 收稿日期:2014-12-04 修回日期:2015-01-09 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 刘俊
  • 基金资助:

    国家质量监督检验检疫总局科研项目(2013IK187,2014IK258).

Determination of 22 acidic dyes in edible packagings by high performance liquid chromatography-tandem mass spectrometry

SU Youzhi1, LIU Jun2, LI Fang1, LEI Hongqin1, LI Yanmei1, LIU Xubin1   

  1. 1. Comprehensive Technical Service Centre of Yili Entry-Exit Inspection and Quarantine Bureau, Yining 835000, China;
    2. Technical Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China
  • Received:2014-12-04 Revised:2015-01-09 Online:2015-04-08 Published:2015-03-30

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221

被引次数

2

摘要：

建立了可食性包装材料中酸性黄23、酸性红18、酸性蓝7等22种酸性染料的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品以乙腈-甲醇(5:5, v/v)提取,采用Strata-X-AW固相萃取柱净化。待测物经Zorbax Eclipse Plus C18柱(100 mm×3.0 mm, 1.8 μm)分离,以乙腈-10 mmol/L乙酸铵为流动相梯度洗脱;采用电喷雾负离子源(ESI-)、多重反应监测(MRM)模式检测;以保留时间和特征离子对(母离子和两个碎片离子)信息比较进行定性,基质匹配外标法定量。22种酸性染料在各自的线性范围内相关系数(r2)均大于0.991;在3种基质(糯米纸、植物胶囊、明胶胶囊)中方法的定量限(以S/N≥10计)为0.1~2.0 mg/kg, 3个加标水平(1、2、10倍定量限)下,回收率为78.4%~109.5%,相对标准偏差(RSD)为4.6%~14.5%。本方法快速简便、准确可靠,适用于可食性包装材料中多种酸性染料的测定。

关键词: 高效液相色谱-串联质谱(HPLC-MS/MS), 固相萃取(SPE), 可食性包装材料, 酸性染料

Abstract:

A method for the simultaneous determination of 22 acidic dyes (acid yellow 23, acid red 18, acid blue 7, etc) in edible packagings was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with acetonitrile-methanol (5:5, v/v), and then cleaned up with Strata-X-AW solid-phase extractor. The analytes were separated on a Zorbax Eclipse Plus C18 column (100 mm×3.0 mm, 1.8 μm) by gradient elution with acetonitrile-10 mmol/L ammonium acetate as the mobile phases. The 22 acidic dyes were determined by electrospray negative ion source (ESI-), and multiple reaction monitoring (MRM) mode. The qualitative analysis was based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions, and the quantitative analysis was carried out by matrix-matched external standard method. The results showed that the calibration curves had good linearity for the 22 acidic dyes, and the correlation coefficients (r2) were larger than 0.991. The limits of quantitation (LOQs, S/N≥10) were in the range of 0.1-2.0 mg/kg in three different matrices (plant capsule, gelatine capsule, oblatum). The average recoveries were in the range of 78.4%-109.5% for the 22 acidic dyes with the relative standard deviations (RSDs) from 4.6% to 14.5% at three spiked levels (1×LOQ, 2×LOQ and 10×LOQ). This method is suitable for the determination of acidic dyes in edible packagings with the characteristics of high accuracy and precision.

Key words: acidic dyes, edible packagings, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), solid-phase extraction (SPE)

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