气相色谱-串联质谱法检测鸭组织中哌嗪的残留  

Determination of piperazine residues in duck tissues by gas chromatography-tandem mass spectrometry

作　　者：王雅娟[1,2] 王波 张杨杨[1,2] 崔璐璐 赵霞[1,2] 郭亚文 谢恺舟[1,2] 张跟喜 戴国俊[1,2] 吴海清 王金玉[1,2] WANG Ya-juan;WANG Bo;ZHANG Yang-yang;CUI Lu-lu;ZHAO Xia;GUO Ya-wen;XIE Kai-zhou;ZHANG Gen-xi;DAI Guo-jun;WU Hai-qing;WANG Jin-yu(College of Animal Science and Technology,Yangzhou University,Yangzhou,Jiangsu 225009,China;Key Laboratory for Animal Genetic,Breeding,Reproduction and Molecular Design of Jiangsu Province,Yangzhou,Jiangsu 225009,China)

机构地区：[1]扬州大学动物科学与技术学院,江苏扬州225009 [2]江苏省动物遗传繁育与分子设计重点实验室,江苏扬州225009

出　　处：《中国兽医学报》2018年第7期1375-1380,共6页Chinese Journal of Veterinary Science

基　　金：国家现代农业产业技术体系资助项目(CARS-42-G23);农业行业标准制定和修订(农产品质量安全)项目[农财发(2013)91号];江苏高校优势学科建设工程资助项目;扬州大学“新世纪人才工程”资助项目

摘　　要：建立了气相色谱-串联质谱法检测鸭组织（肌肉、肝脏、肾脏以及皮肤和脂肪）中哌嗪残留的新方法。样品通过加速溶剂萃取（ASE）和固相萃取（SPE）提取、净化，乙酸酐法衍生化后用气相色谱-串联质谱（GC-MS／MS）检测和确证。采用EI模式，SCAN和SIM扫描定性，Auto SRM结合外标法定量。在定量限（LOQs），50，100,500，1000和2000μg／kg的加标水平上，鸭组织中哌嗪的平均回收率为84．24％-95．49％，相对标准偏差（RSDs）为2．03％-5．30％，日内相对标准偏差为1．72％-5．01％，日间相对标准偏差为2．11％-7．35％。哌嗪在鸭组织的检测限（LODs）为1．4-1．5μg／kg（S／N≥3），LOQs为4.8-5.2μg／kg（S／N≥10），其显著低于最大残留限量（MRL）。此方法灵敏度高。定性、定量准确，适用于鸭组织中哌嗪残留的确证检测。A new method for the determination of piperazine residues in duck tissues（muscle,liver, kidney, skin and fat） by gas chromatography-tandem mass spectrometry was established. Samples were extracted with an accelerated solvent extraction（ASE） apparatus,purified by solid-phase ex- traction（SPE） and derivatized with acetic anhydride,then detected by gas chromatography-tandem mass spectrometry（GC-MS/MS）. Using EI mode, SCAN and SIM scanning qualitative, auto SRM combined with external standard method for quantitative. At spiked levels of the limits of quantification（LOQs）, 50,100,500,1 000 and 2 000 μg/kg,the average recoveries of piperazine in duck tissues were between 2.03% and 5.30% ,with 1.72%-5.01% of the relative standard deviations （RSDs）. The intra-day RSDs were between 84.24% and 95.49%,and the inter-day RSDs were between 2.11% and 7.35%. The limits of detection（LODs） and the LOQs of piperazine were 1.4- 1.5 μg/kg（S/N≥3） and 4.8-5.2 μg/kg（S/N≥10）,respectively,which were considerably lower than the maximum residue limit（MRL）. The method has the advantages of high sensitivity,quantitative and qualitative accuracy, and it is suitable for the detection of piperazine residue in duck tissues.

关 键 词：哌嗪 鸭组织 残留 气相色谱-串联质谱法 

分 类 号：S859.79[农业科学—临床兽医学]