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当前位置: 首页 > 文章 > 气相色谱-串联质谱法检测猪肉中大观霉素和林可霉素残留量 扬州大学学报(农业与生命科学版) 2019 (6) 93-99
Position: Home > Articles > Determination of spectinomycin and lincomycin residues in pork by gas chromatography-tandem mass spectrometry Journal of Yangzhou University(Agricultural and Life Science Edition) 2019 (6) 93-99

气相色谱-串联质谱法检测猪肉中大观霉素和林可霉素残留量

作  者：
丁丽军;沈建新;陈长宽;袁华根;王雅娟;刘楚君;谢恺舟
单  位：
江苏沿海地区农业科学研究所;江苏省兽用生物制药高技术研究重点实验室;扬州大学动物科学与技术学院/教育部农业与农产品安全国际合作联合实验室;常熟市支塘动物防疫站
关键词：
猪肉;大观霉素;林可霉素;残留检测;气相色谱-串联质谱法
摘  要：
为建立气相色谱-串联质谱法检测猪肉中大观霉素和林可霉素残留量的方法,猪肉通过加速溶剂萃取(ASE350), 0.01 mol·L~(-1)磷酸二氢钾缓冲溶液提取,过HLB [3 mL·(60 mg)~(-1)]固相萃取净化,所得净化液经过浓缩后,用正己烷复溶,在双(三甲基硅烷基)三氟乙酰胺(BSTFA)和乙腈条件下衍生,衍生产物用气相色谱-串联质谱(GC-MS/MS)确证和定量检测,色谱柱为TG-5MS (30.0 m×0.25 mm, 0.25μm),采用EI模式,全扫描(SCAN)定性,选择反应监测(Auto SRM)结合外标法定量。结果表明:猪肉中大观霉素和林可霉素分别在5.7～600.0和6.2～200.0μg·kg~(-1)添加范围内,平均回收率分别为80.02%～87.21%和80.17%～85.66%,相对标准偏差(RSD)分别为1.59%～2.61%和1.26%～2.71%,日内RSD分别为2.29%～3.73%和2.61%～4.59%,日间RSD分别为3.98%～5.08%和3.27%～6.07%。猪肉中大观霉素和林可霉素检测限分别为2.6和3.1μg·kg~(-1)(S/N≥3),定量限分别为5.7、6.2μg·kg~(-1)(S/N≥10)。此方法灵敏度高,定性、定量准确,适用于猪肉中大观霉素和林可霉素残留的确证检测。
译  名：
Determination of spectinomycin and lincomycin residues in pork by gas chromatography-tandem mass spectrometry
作  者：
DING Lijun;SHEN Jianxin;CHEN Changkuan;YUAN Huagen;WANG Yajuan;LIU Chujun;XIE Kaizhou;Jiangsu Provincial Key Laboratory of Veterinary Bio-Pharmaceutical High Tech Research;Changshu Zhitang Animal Epidemic Prevention Station;Institute of Agricultural Sciences in Jiangsu Coastal Areas;Joint International Research Laboratory of Agriculture & Agri-Product Safety, the Ministry of Education/College of Animal Science and Technology, Yangzhou University;
关键词：
pork;;spectinomycin;;lincomycin;;residues determination;;GC-MS/MS
摘  要：
A new method for the determination of spectinomycin and lincomycin residues in pork by gas chromatography-tandem mass spectrometry was established. Pork tissues was extracted by accelerated solvent extraction(ASE350) with 0.01 mol·L~(-1) potassium dihydrogen phosphate buffer solution, purified with HLB [3 mL·(60 mg)~(-1)] solid-phase extraction. The purified liquid was concentrated and reconstituted with n-hexane. The reconstituted sample was derivatized with BSTFA and acetonitrile. The derivative product was confirmed and quantified by gas chromatography-tandem mass spectrometry(GC-MS/MS), using TG-5 MS(30.0 m×0.25 mm, 0.25 μm) column. 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. At spiked levels of the 5.7-600.0 and 6.2-200.0 μg·kg~(-1), the average recoveries of spectinomycin and lincomycin in pork were 80.02%-87.21%, 80.17%-85.66%, with the relative standard deviation(RSD) were 1.59%-2.61%, 1.26%-2.71%. The intra-day RSD were 2.29%-3.73%, 2.61%-4.59%, and the inter-day RSDs were 3.98%-5.08%,3.27%-6.07%,respectively.The limit of detection(LOD)and the limit of quantiation(LOQ)of spectinomycin and lincomycin were 2.6,3.1μg·kg-1(S/N≥3)and 5.7,6.2μg·kg-1(S/N≥10),respectively.The method has the advantages of high sensitivity,quantitative and qualitative accuracy,and it is suitable for the detection of spectinomycin and lincomycin residues in pork.

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