快速分散固相萃取-平行液相色谱-串联质谱法同时测定炸鸡食品中26种性激素  

Simultaneous Determination of 26 Sex Hormones in Fried Chicken Food by QuEChERS Combined with Parallel Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄永辉 HUANG Yonghui(Fujian Inspection and Research Institute for Product Quality,National Quality Supervision and Testing Center for Processed Food,Fuzhou 350002,China)

机构地区：[1]福建省产品质量检验研究院,国家加工食品质量检验检测中心,福建福州350002

出　　处：《食品科技》2024年第5期314-320,共7页Food Science and Technology

基　　金：国家市场监督管理总局科技计划项目(2021MK054)。

摘　　要：采用平行液相色谱-串联质谱结合快速分散固相萃取技术,建立了同时测定炸鸡食品中26种性激素残留量的方法。样品以乙腈(水)超声提取,100 mg十八烷基硅烷(C_(18))和100 mg乙二胺-N-丙基硅烷粉末净化,浓缩后以50%甲醇复溶。以Waters ACQUITY UPLC BEH C_(18)为色谱柱,甲醇-2 mmol/L乙酸铵含0.01%氨水溶液为流动相进行梯度洗脱,电喷雾-正负离子切换、多反应监测模式进行测定,基质匹配标准曲线外标法定量。方法学验证表明,在1.0~50.0 μg/L的范围内,26种性激素的线性较好,相关系数(R^(2))均大于0.999,该方法的检出限为0.3~1.0 μg/kg,定量限为1.0~3.0 μg/kg。在炸鸡腿、烤翅和炸鸡块基质中分别进行3水平6平行的加标回收实验,26种性激素的回收率为78.9%~105.3%,相对标准偏差为3.1%~8.4%。所建立的方法简单高效、准确度好、重现性高,适用于炸鸡食品中26种性激素的同时测定。A method for the simultaneous determination of 26 sex hormone residues in fried chicken food was developed using parallel liquid chromatography-tandem mass spectrometry (UPLC/UPLC-MS/MS) combined with quick,easy,cheap,effective,rugged,and safe (QuEChERS).The samples were extracted with acetonitrile(waters),cleaned-up by 100 mg of octadecylsilane (C_(18)) and 100 mg of ethylenediamine-N-propylsilane powder,concentrated and reconstituted in 50% methanol,and then analyzed by the gradient elution on a Waters ACQUITY UPLC BEH C_(18) column,with the mobile phases of methanol-2 mmol/L ammonium acetate containing 0.01% ammonia,and the separation was performed by electrospray ionization in positive-negative ionization switching,and the electrochemical separation with the mobile phases of electrochemistry,electrochemical analysis,and electrophoresis.The determination was carried out in electrospray-positive and negative ion switching,multiple reaction monitoring (MRM) mode,and quantified by matrix-matched standard curve external standard method.The method validation showed that the linearity of the 26 sex hormones was good in the range of 1.0–50.0 μg/L with the correlation coefficients (R~2) greater than 0.999,and the limits of detection (LODs) of the method were in the range of 0.3–1.0 μg/kg,and the limits of quantification (LOQs) were in the range of 1.0–3.0 μg/kg.The recoveries of 26 sex hormones ranged from 78.9% to 105.3% with the relative standard deviations (RSDs) of 3.1% to 8.4%.The established method is simple,efficient,accurate,reproducible and suitable for the simultaneous determination of 26 sex hormones in fried chicken food.

关 键 词：快速分散固相萃取 平行液相色谱-串联质谱 炸鸡 性激素 

分 类 号：TS207.5[轻工技术与工程—食品科学]