色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1147-1154.DOI: 10.3724/SP.J.1123.2011.01147

• 研究论文 • 上一篇    下一篇

超快速液相色谱-串联质谱法测定黄酒和葡萄酒中山梨酸等9种防腐剂和甜味剂

陈晓红, 赵永纲, 姚珊珊, 李小平, 金米聪*   

  1. 宁波市疾病预防控制中心 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010
  • 收稿日期:2011-09-14 修回日期:2011-10-11 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 金米聪,博士,研究员,主要从事食品安全的检测技术研究. Tel: (0574)87274559
  • 基金资助:

    浙江省医药卫生科学研究基金项目(2010KYB098,2011RCB033)和宁波市自然科学基金项目(2010A610010).

SSimultaneous determination of nine preservatives and sweeteners in yellow wine and wine by ultrafast liquid chromatography-tandem mass spectrometry

CHEN Xiaohong, ZHAO Yonggang, YAO Shanshan, LI Xiaoping, JIN Micong*   

  1. Ningbo Municipal Center for Disease Control and Prevention, Ningbo Key Laboratory of Poison Research and Control, Ningbo 315010, China
  • Received:2011-09-14 Revised:2011-10-11 Online:2011-12-28 Published:2012-01-15

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摘要： 建立了一种专属、灵敏的同时测定黄酒和葡萄酒中安赛蜜、糖精、甜蜜素、阿斯巴甜、苯甲酸、山梨酸、甜菊糖苷、纽甜和脱氢乙酸等9种防腐剂和甜味剂的超快速液相色谱-串联质谱(UFLC-MS/MS)分析方法。不同类型的黄酒和葡萄酒经纯水稀释后,以乙腈和0.01%三氟乙酸-2.5 mmol/L乙酸铵水溶液为流动相,采用梯度洗脱方式在Shim-pack XR-ODSII色谱柱(100 mm×2.0 mm, 2.2 μm)上进行分离,以电喷雾负离子多反应监测(MRM)模式进行质谱分析。实验表明,9种防腐剂和甜味剂在检测范围内均具有良好的线性关系(r2＞0.998);方法的检出限(以信噪比大于3计)为0.03～15.0 μg/L,定量限(以信噪比大于10计)为0.1～50.0 μg/L;在黄酒中的回收率为96.2%～100.5%,相对标准偏差(RSDs)为0.6%～5.4%;在葡萄酒中的回收率为96.0%～104.0%, RSDs为0.7%～4.8%。同时研究了这9种防腐剂和甜味剂的二级质谱特征,阐释了其二级质谱裂解途径。本方法灵敏度高、重现性好、分析速度快,可用于黄酒和葡萄酒中防腐剂和甜味剂的快速确证检测。

关键词: 超快速液相色谱-串联质谱法, 防腐剂, 黄酒, 葡萄酒, 甜味剂

Abstract: A sensitive and selective analytical method based on ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) was developed for the simultaneous determination of nine preservatives and sweeteners in yellow wine and wine. After the sample was diluted by pure water, the UFLC separation was performed on a Shim-pack XR-ODSII column (100 mm×2.0 mm, 2.2 μm) with a linear gradient elution program of acetonitrile-ammonium acetate(AmAc, 2.5 mmol/L)-trifluoroacetic acid (TFA, 0.01%, v/v) aqueous solution as the mobile phase. Electrospray ionization was applied and operated in the negative multiple reaction monitoring (MRM) mode. The results showed that the limits of detection (LODs, S/N>3) for the nine analytes were in the range of 0.03~15.0 μg/L, and the limits of quantitation (LOQs, S/N>10) were in the range of 0.1~50.0 μg/L. The calibration curves showed good linearity for the nine analytes in their detection ranges, and the correlation coefficients (r2) were larger than 0.998. The recoveries were between 96.2% and 100.5% with the relative standard deviations (RSDs) of 0.6%~5.4% for yellow wine, and between 96.0% and 104.0% with the RSDs of 0.7%~4.8% for wine. Additionally, the mass spectral characterizations of the nine food additives were studied and the fragmentation pathways were speculated. The method is sensitive, reproducible and adaptable to the simultaneous rapid determination of the nine food additives in different yellow wine and wine samples.

Key words: wine, preservative, sweetener, ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS), yellow wine