高效液相色谱-电化学阵列检测器检测10种磺胺药物在鸡肉中的残留  

Simultaneous Determination of Ten Sulfa Drugs in Chicken Meatby High Performance Liquid Chromatography- Coulometric Array Detector

作　　者：李曙光[1] 赵静玫[1] 王文霞[1] 金郁[1] 杜昱光[1] 

机构地区：[1]中国科学院大连化学物理研究所,大连116023

出　　处：《分析化学》2005年第4期442-446,共5页Chinese Journal of Analytical Chemistry

摘　　要：建立了一步有机溶剂提取、HPLC分离、多孔石墨电极阵列检测器检测10种磺胺类药物在鸡肉中残留量的方法.采用乙腈-氯仿混合液(乙腈∶氯仿=10∶1)提取,10种磺胺药物的提取收率均大于50%;研究了磺胺类药物在多孔石墨电极上的氧化还原特征,确定检测电势为455,560,630,670和710 mV;优化了HPLC分离条件,Hypersil BDS C-18色谱柱,pH 5、30 mmol/L磷酸二氢钠、8.5%～37.5%乙腈(V/V)线性梯度洗脱,40 min内实现10种磺胺药物的基线分离,鸡肉中提取的杂质不干扰样品分离;方法的检出限(S/N=3)为磺胺二甲异喔唑(SIA)40 μg/kg及磺胺(SA)、磺胺嘧啶(SDZ)、磺胺甲基嘧啶(SMR)、磺胺二甲基嘧啶(SMZ)、磺胺吡啶(SPD)、磺胺噻唑(STZ)、磺胺甲噻二唑(SMTZ)、磺胺氯哒嗪(SCP)和磺胺甲基异喔唑(SMX)等分别为20 μg/kg.在0.1～2.0 mg/L浓度范围内各磺胺类药物与其响应信号呈现良好的线性关系,相关系数(r)均大于0.9978;电极再生方法简单,可实现在线清洗,适用于食用畜禽产品中磺胺类药物残留量的分析.One-step extraction and high performance liquid chromatography (HPLC) with coulometric porous graphite electrode array detector method have been developed for the determination of ten sulfa drugs residues in chicken meat. The extraction recoveries of the ten sulfa drugs are higher than 50% with mixture of acetonitrile and chloroform ( acetonitrile : chloroform is 10:1). The redox characteristics of the ten sulfa drugs on porous graphite electrode have been studied, and then the potential for detecting the sulfa drugs is fixed on 455,560,630,670 and 710 mV on electrodes in series. The ten analytes have been separated very well on Hypersil BDS C-18 column with mobile phases containing acetonitrile and 30 mmol/L NaH2PO4 ( pH 5), and with a linear gradient eluting program of acetonitrile from 8. 5% to 37.5% ( V/V) in 40 minutes. The contaminant from chicken meat does not affect the separation of the ten sulfa drugs. The limit of detection is 40 mu g/kg for SIA and 20 mu g/kg for SA, SDZ, SMR, SMZ, SPD, STZ, SMTZ, SCP, and SMX in chicken meat. There are good linear correlations between the peak areas and concentrations of the ten sulfa drugs, the linear range is 0. 1 similar to 2. 0 mg/L and the correlation coefficients are above 0. 99. The electrode recovery is simple and can realize on-line cleanout. This method using HPLC-coulometric array detector is reproducible, and sensitive enough for the determination of sulfa drugs in chicken meat. It is easy to perform.

关 键 词：阵列检测器 高效液相色谱 鸡肉 电化学 磺胺类药物 磺胺二甲基嘧啶 线性梯度洗脱 磺胺甲基嘧啶 HPLC 石墨电极 磷酸二氢钠 药物残留量 溶剂提取 提取收率 氧化还原 分离条件 基线分离 样品分离 磺胺嘧啶 磺胺噻唑 线性关系 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]