液相色谱-四极杆飞行时间质谱用于快速筛查动物组织中多种激素残留的方法研究和应用

建立了一种采用液相色谱-四极杆飞行时间质谱（LC-Q-TOF/MS）用于快速筛查动物组织中多种激素残留的检测方法。样品通过乙腈和乙酸乙酯分步提取，提取液经增强型脂质去除吸附剂（EMR）净化，盐析后经N-丙基乙二胺（PSA）和官能化聚苯乙烯/二乙烯苯（PEP-2）进一步净化，以0.1%甲酸水?0.1%甲酸乙睛作为流动相进行梯度洗脱，在EclipsePlus-C₁₈（3.0 mm×100 mm，1.8 μm）色谱柱上进行分离，在Q-TOF/MS正离子全扫描模式下采集质谱数据，以保留时间、精确分子质量数、同位素丰度比和二级特征碎片离子定性，待测物准分子离子峰面积定量。结果表明，所有药物在各自浓度范围内线性良好，相关系数大于0.995，在10、50、100 μg/kg添加水平下，平均回收率在70.3%～116.2%之间，相对标准偏差为0.87%～8.97%，方法检测限为1～10 μg/kg，定量限为3～30 μg/kg。该方法通过构建一级精确质量数据库和二级谱库，结合保留时间、精确分子质量数、同位素丰度比和二级特征碎片离子，实现对目标化合物快速筛查和确证，具有简单快速、高灵敏度，高选择性和良好精密度的优势，适用于动物组织多种激素的快速筛查和定量测定。

Study and Application on the Method of Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry for Rapid Screening of Multiple Hormone Residues in Animal Tissues

A method for rapid screening of 32 hormone residues in animal tissues by liquid chromatography quadrupole time of flight mass spectrometry (LC-Q-TOF/MS) was established. Samples were extracted by acetonitrile and ethyl acetate and extracted was purified by enhanced lipid removal adsorbent (EMR). After salting out, extract were further purified by PSA and functionalized polystyrene/two vinyl benzene (PEP-2), with 0.1% formic acid water-0.1% formic acid was used as mobile phase for gradient elution, in Eclipse plus-C₁₈ (3.0 mm×100 mm, 1.8 μm) column on the chromatographic column separation. The mass spectrum data were collected in Q-TOF/MS positive ion full scan mode. The retention time, accurate molecular mass number, isotopic abundance ratio and secondary characteristic fragment ions were used for qualitative analysis, and the excimer ion peak area was used for quantitative analysis. The results showed that all the drugs had good linearity in their respective concentration range, and the correlation coefficients was greater than 0.995. The average recoveries ranged from 70.3% to 116.2% at the addition levels of 10, 50 and 100 μg/kg. The relative standard deviation was 0.87% to 8.97%. The limit of detection was 1～10 μg/kg and the limit of quantification was 3～30 μg/kg. By constructing a first-order accurate mass database and a second-order spectral library, combine with retention time, accurate molecular mass number, isotope abundance ratio and secondary characteristic fragment ions, the method could achieve rapid screening and confirmation of target compounds. It had the advantages of simply, rapidity, high sensitivity, high selectivity and good precision, and was suitable for rapid screening and quantitative determination of multiple hormones in animal tissues.