色谱

色谱 ›› 2013, Vol. 31 ›› Issue (2): 170-173.DOI: 10.3724/SP.J.1123.2012.09035

• 技术与应用 • 上一篇    下一篇

分散固相萃取-高效液相色谱法快速测定果蔬中的6种保鲜剂残留量

林海丹*, 邹志飞, 秦燕, 谢守新, 陈毓芳, 徐娟, 王岚, 陈楚莹   

  1. 广东出入境检验检疫局检验检疫技术中心, 广东 广州 510623
  • 收稿日期:2012-09-24 修回日期:2012-12-01 出版日期:2013-02-28 发布日期:2013-02-05
  • 通讯作者: 林海丹
  • 基金资助:

    国家质检总局公益性行业科研专项(201110019);中国检验检疫科学研究院项目(2009JK011);“十二五”农村领域国家科技计划课题(2011BAD23B05-4);广东省科技基础条件建设项目(粤科财字【2008】658,【2010】185).

Rapid determination of six preservative residues in fruits and vegetables by high performance liquid chromatography using dispersive solid phase extraction

LIN Haidan*, ZOU Zhifei, QIN Yan, XIE Shouxin, CHEN Yufang, XU Juan, WANG Lan, CHEN Chuying   

  1. Inspection and Quarantine Technology Center, Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • Received:2012-09-24 Revised:2012-12-01 Online:2013-02-28 Published:2013-02-05
  • Contact: LIN HAIDAN

PDF

393

被引次数

22

摘要： 建立了采用分散固相萃取-高效液相色谱同时测定果蔬中2,4-滴、噻苯咪唑、乙萘酚、邻苯基苯酚、二苯醚和联苯6种保鲜剂残留量的方法。样品经乙腈提取(同时加入氯化钠和无水硫酸镁),提取液经酸性氧化铝分散固相萃取净化,采用Agilent TC C18色谱柱(250 mm×4.6 mm, 5 μm),以甲醇-0.02 mol/L的磷酸二氢钾溶液(pH 6)作为流动相,流速1.0 mL/min,梯度洗脱,用紫外检测器检测,检测波长为235 nm,外标法峰面积定量。6种保鲜剂在0.5～20 mg/L范围内线性关系良好,相关系数均大于0.99; 6种保鲜剂在样品中添加1、2和10 mg/kg 3个浓度水平的回收率为84.2%～99.1% (n=6),相对标准偏差为1.67%～10.3%;方法的定量限为1 mg/kg。该法简便、准确,适用于果蔬中6种保鲜剂残留量的检测。

关键词: 保鲜剂, 分散固相萃取, 高效液相色谱, 果蔬

Abstract: A dispersive solid phase extraction-high performance liquid chromatographic (HPLC) method was established for the simultaneous determination of 2,4-D, thiabendazole, 2-naphthol, o-phenyl phenol, diphenyl ether and biphenyl in the fruits and vegetables. The samples were vortexed for extraction with acetonitrile containing sodium chloride and anhydrous magnesium sulfate. The acetonitrile extraction was purified by acidic alumina dispersed solid phase extraction. The analysis was performed on an Agilent TC C18 column (250 mm×4.6 mm, 5 μm) and an ultraviolet detector at 235 nm with a mobile phase of methanol-0.02 mol/L (pH 6) potassium dihydrogen phosphate solution, at a flow rate of 1.0 mL/min with gradient elution. Good linearities were observed in the range of 0.5-20 mg/L with correlation coefficients greater than 0.99. The average recoveries of the six preservatives in fruits and vegetables were in the range of 84.2%-99.1% at three spiked levels of 1, 2 and 10 mg/kg (n=6) and the relative standard deviations (RSDs) were in the range of 1.67%-10.3%. The limits of quantification were 1 mg/kg. This method is simple, accurate and suitable for the determination of the six preservatives in fruits and vegetables.

Key words: dispersive solid phase extraction, fruits and vegetables, preservatives, high performance liquid chromatography (HPLC)

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