摘要
建立了高效液相色谱-串联三重四极杆质谱(HPLC-MS/MS)测定水产品中氨苯砜及其代谢物残留量的方法。样品加入D8-氨苯砜内标,经1%氨化乙腈提取,正己烷去脂后,采用MCX阳离子固相萃取柱进行富集和净化,氮吹浓缩至0.2 mL左右。用甲醇和水作为流动相,以CAPCELL PAK C18色谱柱(2.0 mm×100 mm,3μm)进行分离,在质谱多反应监测(MRM)、正离子电离模式下测定,采用内标法定量。氨苯砜和N-乙酰氨苯砜在0.1~5.0μg/kg范围内线性关系良好,相关系数(r^(2))均大于0.99,方法检出限(LOD)为0.1μg/kg,定量下限(LOQ)为0.2μg/kg。以不同类型的水产品为空白基质,在0.2、1.0、2.0μg/kg加标水平下,平均加标回收率为94.0%~109%,相对标准偏差(RSD)为2.7%~11%。用该法对药代实验中获得的阳性肌肉样品进行测定,通过对化合物的保留时间和离子对信息进行鉴别,鉴定出氨苯砜的代谢产物为N-乙酰氨苯砜。该方法的检出限低、精密度好、准确度高,能够实现对不同水产品中氨苯砜残留量的准确定性与定量检测。
It is of great significance to develop novel analysis techniques for simultaneous determination of dapsone and its metabolites in aquatic products,so as to realize the simultaneous supervision of dapsone and its metabolites in aquatic products and the comprehensive control of illegal drug use.In this study,a high performance liquid chromatography-tandem triple quadrupole mass spectrometric(HPLC-MS/MS)method was established for the determination of dapsone and its metabolite residues in aquatic products.In the process of sample pre-treatment,the samples were extracted by using 10 mL 1%ammoniated acetonitrile with dapsone-D8 as the internal standard,followed by fat removal with n-hexane.Meanwhile,MCX cationic solid phase extraction column was used for enrichment and purification.The eluent was concentrated to about 0.2 mL by nitrogen blowing at 45℃,and then fixed with 10%methanol solution to 1 mL.After mixing,the eluent was filtered through a 0. 22 μm aqueous phase membrane into an injection vial for detection by HPLCMS/MS. The separation was carried out on a CAPCELL PAK C18(2. 0 mm × 100 mm, 3 μm)bygradient elution using methanol-water as mobile phases. The quantitative analysis of targetcompounds was performed by the internal standard method under multiple reaction monitoring(MRM)and positive ion ionization modes.The results showed that the calibration curves for dapsone and Nacetyldapsone were linear in the mass concentration range of 0. 1-5. 0 μg/kg, with correlationcoefficients(r^(2))all greater than 0. 99.The limits of detection(LODs)were 0. 1 μg/kg and the limitsof quantitation(LOQs)were 0. 2 μg/kg.The average recoveries at three spiked levels of 0. 2,1. 0,2. 0 μg/kg ranged from 94. 0% to 109%, with relative standard deviations(RSDs)of 2. 7%-11%.The positive muscle samples obtained in the drug substitution experiment were determined,and themetabolite of dapsone was identified as N-acetyl dapsone by identifying the retention time of thecompound and the ion pair information. This method has low detection limit, good precision andhigh accuracy,which could realize the accurate qualitative and quantitative determination of dapsoneresidues in fish,shrimp,crab,shellfish and other aquatic products.
作者
伍姿
黄冬梅
娄晓祎
郑蓉
汤云瑜
张璇
张俊
WU Zi;HUANG Dong-mei;LOU Xiao-yi;ZHENG Rong;TANG Yun-yu;ZHANG Xuan;ZHANG Jun(Key Laboratory of Control of Quality and Safety for Aquatic Products(Shanghai),Fishery Products Quality Inspection and Test Center(Shanghai),Ministry of Agriculture and Rural Affairs,East China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Shanghai 200090,China;School of Food Science,Shanghai Ocean University,Shanghai 201306,China;Ti Testing and Certification Group Co.,Ltd.,Shanghai 200060,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2022年第6期882-888,共7页
Journal of Instrumental Analysis
基金
农业国家、行业标准制定和修订项目(农质标函[2019]77号)
中央公益性科研机构基础研究基金,中国水产科学研究院基本科研业务费资助(2020TD72)。
