摘要
建立了动物肌肉中10种β2-兴奋剂、16种激素共26种促蛋白合成剂的固相萃取样品前处理方法,用同位素内标结合气相色谱-质谱联用法进行分析。动物肌肉经过β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,酶解液通过SLW固相萃取柱浓缩净化,先用甲醇洗脱16种激素,然后用5%氨化乙酸乙酯洗脱10种β2-兴奋剂,后者经过双三甲基硅基三氟乙酰胺＋1%（φ）三甲基氯硅烷衍生后,用GC/MS测定β2-兴奋剂;前者再用SLH固相萃取柱净化,七氟丁酸酐衍生后用GC/MS测定激素。结果表明,SLW固相萃取柱能够很好地分离动物肌肉酶解液中10种β2-兴奋剂、16种激素,结合GC/MS测定,本方法检出浓度为0.5-1.0μg/kg,回收率在68.2%-103.2%之间,相对标准偏差1.5%-12.4%。
A sample pretreatment method has been developed for the multi-residue analysis of 26 types anabolic agents including 10 types agonists and 16 types steroids in animal tissues by gas chromatography-mass spectrometry, based on isotope-labeled internal standards and solid phase extraction. The homogenized animal muscle was hydrolyzed by β-glucuronidase/arylsulfatase, then passed through SLW solid phase extraction column. The steroid fraction was obtained by eluting the column with methanol and the agonist fraction was eluted with 5% ammonia in ethyl acetate. The agonist fraction was derivatized with bis（trimethylsilyl ）trifluoroaeetamide ＋ 1% （m/V） trimethylchlorosilane. The steroid fraction was further cleanuped on a SLH cartridge and the purified residue was derivatized with heptafluorobutyrate. Both fractions were analyzed by gas chromatography-mass spectrometry. The experimental results indicated that the 10 types β2-agonists and 16 types steroids could be separated using SLW solid phase extraction column. The detection limits were 0.5 - 1.0μg/kg, the rates of recovery were 68.2% - 103.2% , and the relative standard deviations were 1.5% - 12.4%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第11期1476-1482,共7页
Chinese Journal of Analytical Chemistry
基金
浙江省卫生厅优秀青年人才基金(No.2006QN007)
浙江省重点科研农业基金(No.2005C22029)
浙江省重大科技攻关基金(No.2005C12007)资助项目
关键词
促蛋白合成剂
β2-兴奋剂
激素
多种残留
气相色谱-质谱
Anabolic agents, β2-agonists, steroids, multi-residue, gas chromatography-mass spectrometry
