HPLC-MS-MS同位素内标法测定火腿中14 种喹诺酮类残留量

建立同时测定火腿中14 种喹诺酮类化合物高效液相色谱串联质谱检测方法。样品采用乙腈提取，乙腈饱和正己烷脱脂，经MAX固相萃取小柱净化，采用高效液相色谱串联质谱多反应监测正离子模式测定，使用同位素内标定量。14 种喹诺酮类检出限为0.6 μg/kg。方法平均回收率在70.0%～115.0%之间，相对标准偏差在1.2%～15.6%之间。该方法前处理简便快速、选择性好、灵敏度高，可作为日常的检测方法在实验室中使用。

Determination of 14 Quinolone Residues in Ham by HPLC-MS-MS with Isotopic Internal Standard

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) was developed for
simultaneous determination of 14 quinolone residues (QNS) in ham. Ham sample was extracted with acetonitrile, defatted
with hexane saturated with acetonitrile and cleaned up by MAX solid phase extraction. The mass spectrometer was operated
in the positive ion mode using select reaction monitoring for qualitative and quantitative analysis. Isotope internal standard
was used for quantitative analysis. The limit of detection of the method was 0.6 μg/kg. Mean recovery rates for 14 QNS in
a negative ham sample spiked at three levels were between 70% and 115%, with RSD ranging from 1.2% to 15.6%. This
method proved to be of simplicity, high sensitivity and good selectivity. It has been used for routine test in our laboratory.