Zhao Haixiang, Liu Haiping, Yan Zaoying
Se Pu. 2014 Mar;32(3):294-8. doi: 10.3724/sp.j.1123.2013.11041.
A multi-residue analytical method based on solid-phase extraction (SPE) with multiwalled 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 redissolved 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.
建立了一种以多壁碳纳米管(MWCNTs)为吸附剂的基于固相萃取(SPE)的多残留分析方法。采用高效液相色谱 - 紫外检测(HPLC - UV)法测定猪肉和鸡肉中的磺胺类药物(SAs)。对净化条件进行了优化。分析物用乙腈提取,并用MWCNTs固相萃取柱净化。提取物用Na2HPO4缓冲液(pH 5.5 - 6.0)复溶后上样,先用丙酮 - 己烷(5:95,v/v)洗涤,然后用丙酮 - 二氯甲烷(1:1,v/v)从柱上洗脱。色谱分离所用的流动相由乙腈和50 mmol/L NaH2PO4的二元混合物组成,体积比为7:3。线性范围为0.01 - 1.00 mg/L,相关系数大于0.998。检测限(S/N = 3)为0.003 mg/L,定量限(S/N = 10)为0.01 mg/L。在0.02 - 0.2 mg/kg的加标范围内,9种SAs的平均回收率超过了70%,相对标准偏差(RSDs)低于8%。本研究表明,MWCNTs固相萃取柱对动物组织或产品中的SAs净化效果良好,该方法简单、准确,适用于SAs残留的定量分析。