建立了分散固相萃取-同位素稀释-高效液相色谱-串联质谱（ dSPE-ID-HPLC-MS／MS）同时测定猪肉中26种β-受体激动剂残留的方法。样品经β-葡萄糖醛苷酶／芳基硫酸酯酶水解12 h 后，用高氯酸沉淀蛋白质，取上清液，调节 pH值为9，用乙腈涡旋提取，分散固相萃取净化。选用具有混合分离模式的新型色谱柱 Poroshell 120 Phenyl-Hexyl（100 mm×2.1 mm，4.0μm）对待测物进行分离，在电喷雾离子（ESI）源正离子模式下以多反应监测（ MRM）模式采集数据并做定性筛查和定量分析。26种待测物在相应的浓度范围内线性关系良好，相关系数均大于0.99，在3个不同浓度的添加水平下，平均回收率为65.3％~108.5％，相对标准偏差（ RSD）为2.7％~13.3％，检出限（ LOD，S／N=3）和定量限（ LOQ，S／N=10）分别为0.03~0.1μg／kg及0.1~1.0μg／kg。该方法成本低廉、灵敏可靠，适用于同时对猪肉产品中26种β-受体激动剂残留进行定性和定量筛查。
A method has been developed and validated for the determination of 26 β-agonists in pork using dispersive solid-phase extraction( dSPE ) coupled with isotope dilution-high per-formance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS). After the samples were hydrolyzed by β-glucuronidase/aryl sulfatase for 12 h,the protein was precipitated with perchloric acid. The analytes were extracted with vortex mixer by acetonitrile after adjusting the pH value to nine,and then the extracts were purified using mixed adsorbent by dSPE. After the separation on a novel mixed-mode column of Poroshell 120 Phenyl-Hexyl( 100 mm × 2. 1 mm,4. 0 μm),the qualitative and quantitative analyses of the 26 analytes were operated by electrospray ionization mass spectrometry in the positive mode using multiple reaction monito-ring( MRM). The correlation coefficients of linear calibration curves were over 0. 99 in the cor-responding concentration ranges. The average recoveries of the 26 β-agonists ranged from 65. 3% to 108. 5%,and the relative standard deviations( RSDs ) were 2. 7%-13. 3% in spiked sample at three levels. The limits of detection( LODs,S/N=3)and the limits of quantification ( LOQs,S/N=10)were 0. 03-0. 1 μg/kg and 0. 1-1. 0 μg/kg,respectively. The method is low cost,sensitive,reliable and suitable for the determination of residues of the 26 β-agonists in pork products.
参考文献
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