高效液相色谱-串联质谱法测定猪肉中8种β-受体激动剂残留

Determination of eight kinds of β-agonist residues in pork by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  β-受体激动剂  残留  猪肉

英文关键词:liquid chromatography-tandem mass spectrometry  β-agonist  residues  pork

中文摘要:

      目的 建立高效液相色谱-串联质谱法(High performance liquid chromatography - tandem mass spectrometery, HPLC-MS/MS)同时测定猪肉中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林、氯丙那林、非诺特罗、妥布特罗和喷布特罗残留量的方法。方法 2 g猪肉样品加入8 mL 0.2 mol/L乙酸钠水溶液和50 μL β-葡萄糖醛甙酶, 37 ℃水浴处理, 过滤后加入高氯酸除蛋白质, 用氢氧化钠调节pH至9.5~10, 25 mL乙酸乙酯分两次提取, 浓缩, 用正己烷除脂, 采用HPLC-MS/MS多反应监测模式检测, 外标法定量。结果 克伦特罗、莱克多巴胺、沙丁胺醇、特布他林的线性范围为0.5～5 μg/kg, 氯丙那林、非诺特罗、妥布特罗和喷布特罗的线性范围为0.25～5 μg/kg, 相关系数均大于0.995, 沙丁胺醇、特布他林、氯丙那林、非诺特罗和喷布特罗的检出限为0.25 μg/kg, 定量限为0.50 μg/kg, 克伦特罗、莱克多巴胺、妥布特罗的检出限为0.15 μg/kg, 定量限为0.25 μg/kg。加标回收率为82%～105%, 相对标准偏差为4.65%~16.18%(n=6)。结论 该方法经济、简便、快速、准确, 适用于猪肉中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林、氯丙那林、非诺特罗、妥布特罗和喷布特罗残留量的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of the clenbuterol, ractopamine, salbutamol, terbutaline, chlorpromazine, fenoterol, tulobuterol and penbutolol residues in pork by high performance liquid chromatography -tandem mass spectrometry (HPLC-MS/MS). Methods The 2 g pork samples were added with 8 mL of 0.2 mol/L sodium acetate aqueous solution and 50 μL of β-glucuronosylase in a water bath at 37 ℃. After filtration, perchloric acid was added to remove protein, and the pH was adjusted to 9.510 with sodium hydroxide, extracted twice with 25 mL ethyl acetate, then concentrated, and degreased with n-hexane, detected by HPLC-MS/MS multiple reaction monitoring mode, and the contents were quantified by external standard method. Results Clenbuterol, ractopamine, salbutamol and terbutaline had good relationships in the range of 0.55 μg/kg(r＞0.9950). Chlorpromazine, fenoterol, tulobuterol and penbutolol had good relationships in the range 0.25～5 μg/kg (r＞0.9950). The limit of detection of salbutamol, terbutaline, chlorpromazine, fenoterol and penbutolol was 0.25 μg/kg, and the limit of quantification was 0.50 μg/kg. The detection limit of clenbuterol, ractopamine, tulobuterol was 0.15 μg/kg, and the quantification limit was 0.25 μg/kg. The recovery rates were 82%105%, and the relative standard deviations were 4.65%16.18%(n=6). Conclusion This method is economical, simple, rapid and accurate, and suitable for the determination of clenbuterol, ractopamine, salbutamol, terbutaline, chlorpromazine, fenoterol, tulobuterol and penbutolol residues in pork.