液相色谱-串联质谱法检测奶制品中9种 β-受体阻断剂药物残留量

Determination of 9 β-blockers residues in dairy products by liquid chromatography-tandem mass spectrometry

中文关键词:  β-受体阻断剂  液相色谱-串联质谱法  奶制品

英文关键词:β-blockers  liquid chromatography-tandem mass spectrometry  dairy products

中文摘要:

      目的 建立同时检测奶制品(牛奶、奶粉、奶酪)中9 种β-受体阻断剂(β-blockers, BBS)残留的液相色谱-串联质谱方法。方法 混合均匀的试样经β-葡糖醛苷酶/芳基硫酸酯酶水解, 乙腈提取, 硅藻土与BondElut分散固相萃取填料双重快速净化后, 利用液相色谱-串联质谱法进行定性定量分析。结果 9 种BBs在0.1~20.0 μg/L线性范围内线性关系良好(r≥0.995); 定量限(limit of quantity, LOQ, S/N≥10), 均达到0.5 μg/kg; 3 个添加水平(0.5、1.0和5.0 μg/kg)下的回收率为89.5%~112.5%; 相对标准偏差(relative standard deviation, RSD)为4.2%~11.5%。结论 该方法快速、准确、灵敏, 可用于奶制品样品中多种BBs残留的同时有效测定。

英文摘要:

      Objective To establish a method to simultaneously detect nine β-blockers (BBs) such as ateenolol, pindolol, acebutolol, metoprolol, carazolol, labetalol, bisoprolol, propranolol and penbutolol in dairy products (milk, milk powder and cheese). Methods The samples were hydrolyzed by β-glucuronidase/aryl sulfatase and extracted with acetonitrile, followed by continuous purification procedure of disperse solid phase extraction (d-SPE) with diatomaceous earth and BondElut cartridge. The analytes were separated by liquid chromatography and determined by liquid chromatography-tandem spectrometry under electrospray ion and multiple reaction monitor (sMRM) mode. Results For the quantification, stable isotope-labelled of the analytes were used as internal standards. Over the linear range of 0.1~20.0 μg/L, the correlation coefficients (r) for each BBs was no less than 0.995. The limits of quantification (limit of quantity, LOQ, S/N≥10) of all analytes were 0.5 μg/kg. Recoveries from the spiked samples at three levels (0.5, 1.0 and 5.0 μg/kg) ranged from 89.5% to 112.5% with the relative standard deviation from 4.2% to 11.5%. Conclusion The proposed method can be used to screen and confirm 9 BBs in a single run, which was effective in residue surveillance and detection of BBs in dairy products.