色谱

色谱 ›› 2014, Vol. 32 ›› Issue (3): 294-298.DOI: 10.3724/SP.J.1123.2013.11041

• 技术与应用 • 上一篇    下一篇

多壁碳纳米管固相萃取净化-高效液相色谱法测定猪肉和鸡肉中的磺胺多残留

赵海香, 刘海萍, 闫早婴   

  1. 河北北方学院应用化学研究所, 河北 张家口 075000
  • 收稿日期:2013-11-21 修回日期:2014-01-08 出版日期:2014-03-08 发布日期:2014-03-04
  • 通讯作者: 赵海香
  • 基金资助:

    河北北方学院应用化学创新团队项目（CXTD1306）；河北北方学院创新人才培育基金（CXRC1302）.

Analysis of sulfonamide residues in pork and chicken by high performance liquid chromatography coupled with solid-phase extraction using multiwalled carbon nanotubes as adsorbent

ZHAO Haixiang, LIU Haiping, YAN Zaoying   

  1. Institute of Applied Chemistry, Hebei North University, Zhangjiakou 075000, China
  • Received:2013-11-21 Revised:2014-01-08 Online:2014-03-08 Published:2014-03-04

PDF

316

被引次数

34

摘要：

建立了多壁碳纳米管为吸附剂的固相萃取净化-高效液相色谱-紫外检测测定猪肉和鸡肉中多种磺胺类药物多残留的方法。样品采用乙腈提取，多壁碳纳米管固相萃取净化，NaH2PO4缓冲溶液（pH 5.5~6.0）溶解上样，5%（v/v）丙酮-正己烷淋洗，丙酮-二氯甲烷（1：1，v/v）洗脱。色谱分离以50 mmol/L NaH2PO4-乙腈（7：3，v/v）为流动相，方法的线性范围为0.01~1.00 mg/L，线性相关系数大于0.998，检出限（LOD）为0.003 mg/L，定量限（LOQ）为0.01 mg/L。在0.02~0.2 mg/kg添加范围内，9种磺胺类药物的回收率高于70%，RSD低于8%，表明多壁碳纳米管对磺胺类药物具有较强的吸附富集能力。该方法简便、准确可用于动物组织及产品中磺胺药物残留的检测。

关键词: 多壁碳纳米管, 高效液相色谱, 固相萃取, 磺胺, 鸡肉, 猪肉

Abstract:

A multi-residue analytical method based on solid-phase extraction (SPE) with multi-walled carbon nanotubes (MWCNTs) as sorbent was developed. The determination of the sulfonamides (SAs) in pork and chicken was carried out by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The clean-up conditions were optimized. The analytes were extracted by acetonitril and cleaned-up by MWCNTs SPE cartridge. The extract was re-dissolved with the Na2HPO4 buffer (pH 5.5-6.0) for loading, and was washed with acetone-hexane (5:95, v/v), then eluted with acetone-dichloromethane (1:1, v/v) from the column. The mobile phase used in the chromatographic separation consisted of a binary mixture of acetonitrile and 50 mmol/L NaH2PO4 with the volume ratio of 7:3. A wide linear range was 0.01-1.00 mg/L with the correlation coefficients above 0.998. The limits of detection (S/N=3) were 0.003 mg/L, and the limits of quantification (S/N=10) were 0.01 mg/L. The average recoveries were over 70% for the nine SAs in the spiked range of 0.02-0.2 mg/kg, with the relative standard deviations (RSDs) lower than 8%. This study indicated that the MWCNTs SPE cartridge is efficient for the clean-up of the SAs in animal tissues or products, and the method is simple, accurate and suitable for the quantification of the SAs residues.

Key words: chicken, high performance liquid chromatography-ultraviolet detection (HPLC-UV), multi-walled carbon nanotubes (MWCNTs), pork, solid-phase extraction (SPE), sulfonamides (SAs)

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