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

Analysis of sulfonamide residues in pork and chicken by highperformance liquid chromatographycoupled with solid-phase extraction usingmultiwalled carbon nanotubes as adsorbent

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50mmol/LNaH2PO4-乙腈（7：3，v/v）为流动相，方法的线性范围为0.01～1.00mg/L，线性相关系数大于0.998，检出限（LOD）为0.003mg/L，定量限（LOQ）为0.01mg/L。在0.02～0.2mg/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。

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 sul-fonamides（SAs）in pork and chicken was carried out by high performance liquid chromatogra-phy-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 Na 2 HPO 4 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 ace-tonitrile and 50 mmol / L NaH 2 PO 4 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 recover-ies 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 car-tridge 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.