首页|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

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

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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(C18)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 ACQUITYUPLC BEHC18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(R2)均大于0.999,该方法的检出限为0.3~1.0μg/kg,定量限为1.0~3.0μg/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.
Simultaneous Determination of 26 Sex Hormones in Fried Chicken Food by QuEChERS Combined with Parallel Liquid Chromatography-Tandem Mass Spectrometry
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(C18)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 C18 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(R2)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.

Quick,easy,cheap,effective,rugged,and safeparallel liquid chromatography-tandem mass spectrometryfried chickensex hormones

黄永辉

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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

快速分散固相萃取 平行液相色谱-串联质谱 炸鸡 性激素

国家市场监督管理总局科技计划项目

2021MK054

2024

食品科技
北京市粮食科学研究所

食品科技

CSTPCD北大核心
影响因子:0.622
ISSN:1005-9989
年,卷(期):2024.49(5)
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