色谱

色谱 ›› 2017, Vol. 35 ›› Issue (11): 1160-1164.DOI: 10.3724/SP.J.1123.2017.07005

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱联用测定水果及果酱中的展青霉素

吕伟超, 申书昌, 王超   

  1. 齐齐哈尔大学分析测试中心, 黑龙江 齐齐哈尔 161006
  • 收稿日期:2017-07-04 出版日期:2017-11-08 发布日期:2014-01-17
  • 通讯作者: 申书昌,E-mail:sscfxzx@163.com
  • 基金资助:

    黑龙江省教育厅基本业务专项（135209221，135109206）.

Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography

LÜ Weichao, SHEN Shuchang, WANG Chao   

  1. Analytical and Testing Center of Qiqihar University, Qiqihar 161006, China
  • Received:2017-07-04 Online:2017-11-08 Published:2014-01-17
  • Supported by:

    Special Research Project of Heilongjiang Province Education Office (Nos. 135209221, 135109206).

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被引次数

2

摘要：

以硅酸镁、硅胶、硅藻土、硫酸钙为原料，加入乙醇研磨成匀浆，干燥，填充于聚丙烯柱管中，制备成新型固相萃取小柱。样品经果胶酶酶解，乙腈提取，固相萃取净化，以C18色谱柱（100 mm×2.1 mm，1.8 μm）为分离色谱柱进行定性、定量分析。流动相为0.8%（体积分数）四氢呋喃水溶液，流速为0.5 mL/min，以276 nm波长进行检测。考察了果胶酶对萃取效果的影响、固相萃取小柱的净化效果及最佳色谱分析条件。在0.1~10 mg/L范围内，展青霉素峰高与质量浓度呈良好的线性关系，相关系数（R2）为1，方法检出限为10.22 μg/kg，样品的加标回收率为86.58%~94.84%，相对标准偏差（RSD）为1.45%~2.28%。实验结果表明，自制固相萃取小柱净化效果好，超高效液相色谱分离效能高，样品测定操作方法简单，结果准确，对水果制品的质量安全控制具有重要的意义。

关键词: 超高效液相色谱, 固相萃取, 水果制品, 展青霉素

Abstract:

With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient (R2) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

Key words: fruit products, patulin (PAT), solid phase extraction (SPE), ultra performance liquid chromatography (UPLC)

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