动物组织中氨苯砜及其代谢产物残留量的液相色谱串联质谱法测定  

Determination of Dapsone and Its Metabolite Residue in Animal Tissue by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：田云[1] 岳振峰[2] 叶卫翔[2] 赵凤娟[2] 侯乐锡[2] 饶丽[2] 郑必胜[1] 

机构地区：[1]华南理工大学轻工与食品学院,广东广州510640 [2]深圳出入境检验检疫局食品检验检疫技术中心,广东深圳518067

出　　处：《分析测试学报》2009年第1期88-92,共5页Journal of Instrumental Analysis

摘　　要：建立了动物组织中氨苯砜及其代谢产物N-乙酰氨苯砜的液相色谱-电喷雾串联质谱检测方法(HPLC-ESIMS/MS)。采用YMC-Pack ProC18(3μm,100mm×2.0mmi.d.)反相色谱柱,以碱性乙腈为提取液,以HLB和MCX固相萃取柱为净化柱,乙腈-水为流动相,梯度洗脱,流速0.3mL/min,以正离子多反应监测模式测定,同位素内标法定量,进样量15μL。方法的定量下限为0.5μg/kg,线性范围为0.5～5.0μg/kg,加标回收率为92%～103%,相对标准偏差为4.8%～11.0%。该法具有灵敏、准确等优点,适用于动物组织中氨苯砜及其代谢产物N-乙酰氨苯砜残留的确证检测。A liquid chromatography tandem mass spectrometry（LC- MS/MS） method was developed for determination of dapsone （DDS） and its metabolite mono-N-acetyl dapsone （MADDS） residues in animal tissue. The sample was extracted by alkalized acetonitrile, and cleaned up by HLB and MCX solid phase extraction column. The extract was separated on a reversed-phase column of YMC-Pack Pro C18（3μm,100mm×2.0mmi.d. ） by using acetonitrile -water as mobile phase with flow rate of 0. 3 mL/min and gradient elution. The quantitation detection was performed on LC - tandem MS by using multiple reaction monitoring（MRM） mode under positive-ion electrospray ionization and emplo- ying Ds-dapsone as an internal isotope standard. The linear plots were obtained for DDS and MADDS between 0.5 and 5.0 μg/kg. The limits of quantitation （LOQ） were both 0.5 μg/kg. The average recoveries of DDS and MADDS from spiked sample at three concentration levels were between 92% and 103% with RSD（n = 10） of 4.8%- 11.0%. The method was sensitive and accurate, and was suitable for the determination and confirmation of dapsone and its metabolite mono-N-acetyl dapsone in animal tissues.

关 键 词：液相色谱串联质谱 氨苯砜 N-乙酰氨苯砜 动物组织 残留 

分 类 号：O657.63[理学—分析化学] O623.83[理学—化学]