气相色谱-串联质谱检测鹅组织中哌嗪残留  

Studies on method for the determination of piperazine in goose tissues by gas chromatography-tandem mass spectrometry

作　　者：赵霞[1,2] 王波 崔璐璐[1,2] 张杨杨 王雅娟[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] 

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

出　　处：《分析试验室》2017年第12期1423-1428,共6页Chinese Journal of Analysis Laboratory

基　　金：国家现代农业产业技术体系项目(CARS-41-G23);农业行业标准制定和修订(农产品质量安全)项[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"项目资助

摘　　要：建立了鹅组织(肌肉、肝脏、肾脏以及皮肤和脂肪)中哌嗪残留的气相色谱-串联质谱检测法。鹅组织经加速溶剂萃取(ASE350),乙腈提取,过Strata-X-C固相萃取小柱净化后的样品在乙酸酐和三乙胺条件下衍生。衍生产物经气相色谱-串联质谱仪(GC-MS/MS)检测,色谱柱为TG-5MS Amine(30 m×0.25 mm i.d.,0.25μm),载气为氦气,进样口和检测器温度均为280℃。采用EI模式,SCAN和SIM扫描定性,Auto SRM结合外标法定量。哌嗪添加量在5.1~2.5×10~3μg/kg范围内,线性关系良好,相关系数为0.9995。在定量限(LOQ:5.1,5.2,5.2,5.2)~2.0×10~3μg/kg的加标水平上,鹅组织中哌嗪的平均回收率为85.2%~95.5%,相对标准偏差(RSD)为1.6%~4.7%,日内RSD为1.2%~5.3%,日间RSD为2.0%~7.7%。检测限(LOD)和定量限(LOQ)分别在1.4~1.6μg/kg(S/N≥3)和5.1~5.2μg/kg(S/N≥10)之间。方法适用于鹅组织中哌嗪残留的检测。The method for the determination of piperazine residues in goose tissues（muscle,liver,kidney,skin and fat） was established using gas chromatography-tandem mass spectrometry（GC-MS/MS）. Goose tissues were extracted by accelerated solvent extraction（ASE350） with acetonitrile,and then purify with Strata-X-C SPE column and the purified samples was derived with acetic anhydride under triethylamine conditions. The derivatives were detected by GC-MS/MS,using TG-5 MS Amine（30 m × 0. 25 mm i. d.,0. 25 μm） column with helium as the carrier gas,with the inlet and detector temperature both at 280 ℃. The experimental method was used by EI mode,with SCAN and SIM scanning for quantitative analysis,and Auto SRM combined with external standard method for quantification. The method showed a good linear relationship over the concentration range of 5. 1 ~2. 5 × 10~3μg/kg（r = 0. 9995）. At spiked levels of the limit of quantification（LOQ： 5. 1,5. 2,5. 2,5. 2） ~ 2. 0 × 10~3μg/kg,the average recoveries of piperazine in goose tissues were 85. 2% ~95. 5%,with relative standard deviations（RSDs） of 1. 6% ~ 4. 7%. The intra-day RSDs and the inter-day RSDs were 1. 2% ~ 5. 3% and 2. 0% ~ 7. 7%,respectively. The limits of detection（LODs） and limits of quantification（LOQs） were in the range of 1. 4 ~ 1. 6 μg/kg（S/N ≥ 3） and5. 1 ~ 5. 2 μg/kg（S/N ≥ 10）,respectively. The method has the advantages of high sensitivity,quantitative and qualitative accuracy,and it was suitable for the detection of piperazine residue in goose tissues.

关 键 词：鹅组织 哌嗪 气相色谱-串联质谱法 残留 

分 类 号：S859.84[农业科学—临床兽医学]