超高效液相色谱-串联质谱法检测动物肌肉组织中19种β-受体激动剂残留

Determination of 19 β-agonists in Animal Muscle Tissues by UPLC-MS/MS

关键词:  肌肉组织  β-受体激动剂  残留  超高效液相色谱-串联质谱

Key words:  muscle tissues  β-agonists  residue  UPLC-MS/MS

摘要:

建立了猪、牛和羊肌肉组织中吡布特罗、西马特罗、特步他林、齐帕特罗、沙丁胺醇、西布特罗、克伦塞罗、克伦丙罗、羟甲基克伦特罗、氯丙那林、莱克多巴胺、克伦特罗、妥布特罗、福莫特罗、溴布特罗、克伦潘特、班布特罗、马布特罗和马喷特罗等19种β-受体激动剂残留检测的超高效液相色谱-串联质谱方法。猪、牛和羊肌肉组织样品用乙腈和异丙醇（8:2，V/V）提取，加入NaCl、Na2SO4和MgSO4盐析去杂质。待测药物经BEH C18色谱柱分离，以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱。同位素内标法和基质匹配标准溶液外标法定量。19种β-受体激动剂在系列浓度范围内呈现良好线性关系，相关系数r2均大于0.99；19种药物在肌肉组织中的检测限为0.25 μg/kg，定量限为0.5 μg/kg。从0.5、1和5 μg/kg三个添加浓度检测结果可以看出，19种药物的回收率为73.7%～114.1%，批内批间相对标准偏差均小于20%。结果表明，该方法简便快捷、灵敏度高、定性准确，适用于该类药物残留的检测。

Abstract:

A UPLC-MS/MS method was established for the determination of pirbuterol、cimaterol、terbutaline、zilpaterol、salbutamol、cimbuterol、clencyclohexerol、clenproperol、hydroxymethyl clenbuterol、clorprenaline、ractopamine、clenbuterol、tulobuterol、formoterol、brombuterol、clenpenterol、bambuterol、mabuterol and mapenterol residue in pig、cattle and goat muscle tissues. Sample was extracted by acetonitrile and isopropanol (8：2,V/V) and was spiked NaCl, Na2SO4 and MgSO4. The separation of β-agonists was performed with BEH C18 column and the gradient elutinon solvent of acetonitrile(0.1% formic acid) and water(0.1% formic acid) at a flow rate of 0.3 mL/min. The method was quantified by internal standard method and matrix matched standard solution external method, The calibration curves were good linear between serial concentrations，the correlation coefficient r2＞0.99. The limits of detection of 19 β-agonists in muscle tissues were 0.25 μg/kg, and the limit of quantification was 05 μg/kg. The average recoveries obtained from spiked muscle tissues at three concentrations of 0.5,1 and 5 μg/kg were in the ranged of 73.7%～114.1%. The intra- and inter-batch variation coefficients were both less than 20%. This method was simple and rapid, high sensitivity and qualitative accurately.