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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
引用本文:赵海香,刘海萍,闫早婴.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[J].色谱,2014,32(3):294-298.
作者姓名:赵海香  刘海萍  闫早婴
作者单位:河北北方学院应用化学研究所, 河北 张家口 075000
基金项目: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)
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(pH5.5~6.0)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:固相萃取  高效液相色谱  磺胺  猪肉  鸡肉  多壁碳纳米管
收稿时间:2013-11-21

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.Analysis of sulfonamide residues in pork and chicken by high performance liquid chromatography coupled with solid-phase extraction using multiwalled carbon nanotubes as adsorbent[J].Chinese Journal of Chromatography,2014,32(3):294-298.
Authors:ZHAO Haixiang;LIU Haiping;YAN Zaoying
Affiliation:Institute of Applied Chemistry, Hebei North University, Zhangjiakou 075000, China
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.
Keywords:solid-phase extraction (SPE)  high performance liquid chromatography-ultraviolet detection (HPLC-UV)  sulfonamides (SAs)  pork  chicken  multi-walled carbon nanotubes (MWCNTs)
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