色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱分析柑橘类水果中残留的苯丁锡

刘志杏1, 郭平2, 王远兴1*, 占春瑞2*, 左海根2   

  1. 1.State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047, China; 2.Jiangxi Entry-Exit Inspection and Quarantine Bureau, Nanchang 330002, China
  • 收稿日期:2009-02-27 修回日期:2009-03-27 出版日期:2009-11-30 发布日期:1981-12-25
  • 通讯作者: 王远兴，占春瑞

Determination of fenbutatin oxide residue in orange products by gas chromatography

LIU Zhixing1, GUO Ping2, WANG Yuanxing1*, ZHAN Chunrui2*, ZUO Haigen2   

  1. 1.State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047, China; 2.Jiangxi Entry-Exit Inspection and Quarantine Bureau, Nanchang 330002, China
  • Received:2009-02-27 Revised:2009-03-27 Online:2009-11-30 Published:1981-12-25
  • Contact: WANG Yuanxing，ZHAN Chunrui

PDF

687

被引次数

23

摘要： 建立了气相色谱-火焰光度检测器测定柑橘类水果中苯丁锡残留量的检测方法。样品在酸性条件下经丙酮及正己烷萃取并浓缩,用正己烷溶解残渣,经乙基溴化镁衍生后,采用硅胶固相萃取柱净化,正己烷-二氯甲烷(体积比为4:1)混合液洗脱,用毛细管气相色谱-火焰光度检测器(锡滤光片: 610 nm)测定,外标法定量。结果表明: 该方法的线性范围为0.2～2.0 mg/L,相关系数r≥0.9995;当阴性脐橙样品中加标水平为0.1～0.4 mg/kg时,苯丁锡的回收率为79.6%～109.6%,相对标准偏差为3.60%～9.05%,方法的检出限为0.1 mg/kg。该方法重复性好,灵敏度高,完全满足国内外柑橘类水果中苯丁锡残留分析的要求。

关键词: 苯丁锡, 残留, 柑橘 , 气相色谱

Abstract: An analytical method for the determination of fenbutatin oxide (FBT) residue in oranges by capillary gas chromatography-flame photometric detection (GC-FPD) was developed. The FBT was extracted with acetone-acetic acid (99:1, v/v) and hexane, filtered and evaporated by nitrogen evaporator in a water bath at 35 ℃. The residue was dissolved in hexane. The FBT in the solvent was derivatized with ethyl magnesium bromide for 15 min, 1 mol/L hydrochloride was added, the supernatant was collected and the solvent was evaporated to get dry supernatants, then the supernatant was dissolved in hexane and cleaned up with a silica solid phase extraction column, eluted with 5 mL hexane-dichloromethane (4:1, v/v), determined by GC. The standard curve was linear in the range of 0.2~2.0 mg/L. The correlation coefficients (r) were more than 0.9995, the average recoveries were 79.6%~109.6% with the relative standard deviations (RSDs) of 3.60%~9.04% at the spiked levels of 0.1~0.4 mg/kg, and the detection limit of fenbutatin oxide was 0.1 mg/kg. This method is suitable for the analysis of fenbutatin oxide residue in orange products.

Key words: fenbutatin oxide (FBT), orange , residue, gas chromatography (GC)