色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1155-1159.DOI: 10.3724/SP.J.1123.2011.01155

• 研究论文 • 上一篇    下一篇

高效液相色谱串联质谱法检测腰果中黄曲霉毒素

毕瑞锋1,2*, 范志先1, 付萌2   

  1. 1. 青岛科技大学化工学院, 山东 青岛 266042; 2. 诺安检测服务有限公司, 山东 青岛 266002
  • 收稿日期:2011-06-28 修回日期:2011-07-23 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 毕瑞锋,硕士研究生,研究方向为食品安全检测. Tel: (0532)83816633/890,

Determination of aflatoxins in cashew by high performance liquid chromatography-tandem mass spectrometry

BI Ruifeng1,2*, FAN Zhixian1, FU Meng2   

  1. 1. College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China; 2. Sino Analytica Limited, Qingdao 266002, China
  • Received:2011-06-28 Revised:2011-07-23 Online:2011-12-28 Published:2012-01-15

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摘要： 建立了腰果中4种黄曲霉毒素的高效液相色谱-串联质谱检测方法(HPLC-MS/MS)。样品用甲醇-水(8:2, v/v)溶液提取后用弗罗里硅土柱净化,5 mL丙酮-水-甲酸溶液(96:3.5:0.5, v/v/v)洗脱,氮吹至干,1 mL甲醇定容;在资生堂MG C18色谱柱(100 mm×3.0 mm, 3 μm)上梯度洗脱分离,然后采用电喷雾离子化三重四极杆串联质谱测定。实验结果表明,4种黄曲霉毒素在各自的线性范围内峰面积与其质量浓度线性关系良好,相关系数(r2)大于0.997;检出限(信噪比为3)为0.009～0.04 μg/kg,定量限(信噪比为10)为0.03～0.12 μg/kg;平均回收率为63.0%～78.5%,相对标准偏差为2.8%～9.1%,均符合痕量分析的要求。评价了基质效应,信号抑制/增强值为88.8%～99.4%,说明净化后的基质效应较小。该方法简单快速、准确可靠,可用于腰果中黄曲霉毒素的检测。

关键词: 高效液相色谱-串联质谱法, 黄曲霉毒素, 腰果

Abstract: A determination method of four aflatoxins in cashew was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Sample was extracted with methanol-water (8:2, v/v) solution and a cleanup procedure with florisil column was adopted, after eluting with 5 mL acetone-water-formic acid (96:3.5:0.5, v/v/v) solution, the eluate was dried under N2 and the residue was redissolved with methanol. Four aflatoxins were separated in MG C18 column and detected by tandem mass spectrometry. The method was validated, the good correlation coefficients (r2>0. 997) of four aflatoxins were obtained within their respective linear ranges, the limits of quantification were less than 0. 2 μg/kg, mean recoveries were between 63. 0% and 78. 5%, relative standard deviations (RSDs) varied from 2. 8% to 9. 1%, meeting the requirements of trace assay. The sample preparation is simple, fast, and inexpensive, this method can be applied for the determination of aflatoxins in cashew.

Key words: cashew, florisil column, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), aflatoxin