凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱法检测猪肉中9种β2-受体激动剂激素残留

摘要

A gel permeation chromatography-solid phase extraction-rapid resolution liquid chromatography-tandem mass spectrometry (GPC-SPE-RRLC-MS/MS) method for the determination of 9 β2-agonist hormones including salbutamol, terbutaline, cimeterol, fenoterol, clenbuterol, ractopamine, clorprenaline, tulobuterol and penbutolol in pork has been developed. Pork samples were hydrolyzed with β-glucuronidase/arylsulfatase, extracted with tert-butyl methyl ether under ultrasonic incubation and cleaned up using gel permeation chromatography followed by solid phase extraction on an HLB column. After RRLC gradient elution separation on an Agilent Plus C18 column using methanol-water containing 0.1% formic acid as a mobile phase, the pooled eluate was qualitatively and quantitatively determined by tandem mass spectrometry under multi-reaction monitoring (MRM) mode. The limits of detection of this method were 0.1–0.3 μg/kg, and the developed calibration curves revealed excel ent linearity with correlation coefficients larger than 0.996. At spiked levels of 0.3, 2.0 μg/kg and 5.0 μg/kg, average recovery rates of 9 β2-agonist hormones were in the range of 79.35%–109.80%, with RSDs between 2.12% and 9.11%. This method was sensitive, reproducible, accurate and applicable for the determination of β2-agonist hormones in pork.%建立凝胶净化色谱-固相萃取-超快速液相色谱-串联质谱(GPC-SPE-RRLC-MS/MS)测定猪肉中β2-受体激动剂激素残留(沙丁胺醇、西马特罗、特布他林、克伦特罗、莱克多巴胺、氯丙那林、喷布特罗、妥布特罗、非诺特罗)的方法。试样经β-盐酸葡萄糖醛苷酶/芳基硫酸酯酶酶解，叔丁基甲醚超声提取，凝胶净化色谱和HLB柱净化，以甲醇-0.1%甲酸溶液为流动相，经AgilentPlusC18柱分离后进行RRLC-MS/MS多反应监测扫描模式分析检测。方法线性相关系数r＞0.996，检出限为0.1～0.3μg/kg，在0.3、2.0、5.0μg/kg3种添加水平的平均回收率为79.35%～109.80%；相对标准偏差为2.12%～9.11%。该方法灵敏度高、重现性好、定性定量准确，适用猪肉样品检测。