液相色谱法检测水产品中亚甲蓝及其代谢物残留  

Determination of Methylene Blue and Its Metabolites in Aquatic Products by High Performance Liquid Chromatography

作　　者：杨方[1,2] 范克伟[3] 刘正才[1] 林永辉[1] 陈健[1] 林雁飞 胡小钟 陈国南[2] 

机构地区：[1]福建出入境检验检疫局,福州350001 [2]食品安全分析与检测技术教育部重点实验室(福州大学),福州350003 [3]福建农林大学动物科学学院,福州350003 [4]湖北出入境检验检疫局,武汉430022

出　　处：《分析化学》2009年第4期517-521,共5页Chinese Journal of Analytical Chemistry

基　　金：“十一·五”国家科技支撑计划项目(No.2006BAK02A08);福建省科技攻关重点项目(No.2006Y0002)资助

摘　　要：建立了液相色谱同时检测水产品中亚甲基蓝及其代谢物天青A、天青B、天青C残留的方法并用于样品检测。试样中残留的药物以含离子对试剂对甲苯磺酸的乙酸铵缓冲液-乙腈提取,二氯甲烷反萃,MCAX固相萃取小柱净化,液相色谱测定。对提取、净化及仪器分离分析条件进行了探讨,对亚甲基蓝在分析过程的稳定性进行了研究。水产品中4种化合物在0.005～0.50mg/kg范围内线性关系良好,相关系数为0.9946～0.9978。在0.005～0.5mg/kg浓度范围内,平均加标回收率为75.9%～93.2%;相对标准偏差为3.3%～11.9%;AZA、AZB、AZC、MB的检出限分别为1.27、0.98、1.48和1.33μg/kg。方法稳定可靠,可满足水产品中亚甲基蓝及其代谢物的检测需要。An effective high performance liquid chromatographic method has been developed for the determination of dye methylene blue （MB） and its metabolites azure A （ AZA）, azure B （ AZB）, azure C （AZC） in aquatic products, and applied to samples of incurred samples, which had been dosed with methylene blue. Based on ion-pair formation with p-toluenesulfonic acid, the analytes were extracted from homogenised tissue using aeetonitrile, partitioned against methylene dichloride , and purified with a mixed-mode cation exchange solid phase extraction cartridges. The linear range was 0. 005 - 0.50 mg/kg in spiked samples and the correlation coefficients were 0. 9946 - 0. 9978. The average recoveries and the relative standard deviation ranged from 75.9% to 93.2% and 3.3% to 11.9% , respectively, in spiked tissue samples at concentration levels ranging from 0. 005 to 0.5 mg/kg of each analytes. The limits of detection（LOD） of AZA, AZB, AZC and MB were 1.27, 0.98, 1.48 and 1.33 μg/kg, respectively. This method is suitable for the determination of methylene blue and its metabolites residues in aquactic products and pharmacokinetics study.

关 键 词：亚甲基蓝 天青 代谢物 水产品 液相色谱 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]