分子印迹固相萃取/毛细管电泳法检测牛奶中头孢噻肟残留  被引量:10

Determination of Cefotaxime Residue in Milk by Molecular Imprinted Solid Phase Extraction/Capillary Electrophoresis

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作  者:陈玎玎[1] 何东旭[2] 祁克宗[2] 陆翠珍[1] 

机构地区:[1]安徽农业大学生物技术中心,安徽合肥230036 [2]安徽农业大学动物科技学院,安徽合肥230036

出  处:《分析测试学报》2012年第10期1334-1338,共5页Journal of Instrumental Analysis

基  金:国家"十一五"科技支撑项目子项目(2006BAK02A08-4);安徽高校省级自然科学研究项目(KJ2011B065)

摘  要:采用分子印迹技术,以头孢噻肟(CTX)为模板分子,α-甲基丙烯酸(MAA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂合成了头孢噻肟分子印迹聚合物(CTX-MIP)。以该分子印迹聚合物为固相萃取柱填料,毛细管电泳进行检测,建立了分子印迹固相萃取/毛细管电泳检测牛奶中头孢噻肟残留的方法。结果表明,CTX-MIP对CTX具有较高的选择性,萃取效果良好。该方法在CTX为5~100 mg/L范围内呈良好线性,相关系数(r2)为0.999 4;3种不同加标水平(10、50、100 mg/L)的回收率分别为78%、84%、86%,相对标准偏差(RSD)为3.5%~4.5%,检出限(LOD,S/N≥3)为98.52μg/L,定量下限(LOQ,S/N≥10)为329.0μg/L,符合兽药残留分析的要求。A molecularly imprinted polymer for cefotaxime (CTX - MIP) was synthesized by the molecular imprinting technique using cefotaxime (CTX) as template molecule, a-methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as cross linking agent. By using the cefotaxime molecularly imprinted polymer as sorbent in solid-phase extraction column, a molecularly imprinted solid phase extraction -capillary electrophoresis (MISPE -HPCE) method was developed for the determination of cefotaxime residue in milk. The results showed that cefotaxime imprinted polymer exhibited a higher selectivity to cefotaxime compared with that of the non-imprinted polymer. The linear range of cefotaxime was in the range of 0. 5 - 100 mg/L, and the correlation coefficient was 0. 999 4. The recoveries at three spiked concentration levels of 10, 50, 100 mg/L were 78% , 84% and 86% , respectively, with RSDs of 3.5% - 4. 5%. The limit of detection ( LOD, S/N≥3) and the limit of quantitation(LOQ, S/N≥3) were 98.52 μg/L and 329. 0 μg/L, respectively. The method could meet the requirements for veterinary drug residue analysis.

关 键 词:分子印迹固相萃取 毛细管电泳 头孢噻肟 牛奶 

分 类 号:O657.8[理学—分析化学] S859.796[理学—化学]

 

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