基于UPLC-Q/Orbitrap高分辨质谱多目标快速筛查鱼肉中30种蛋白同化激素及糖皮质激素

摘要/Abstract

摘要： 建立了基于超高效液相色谱-四级杆/静电场轨道阱高分辨质谱联用技术快速筛查和确证鱼肉中30种蛋白同化激素及糖皮质激素的分析方法。鱼肉样品用80%乙腈水溶液（含0.2%甲酸）提取，离心，Oasis PRiME HLB固相萃取柱净化，氮吹后复溶。采用Waters Acquity BEH C18 色谱柱（2.1 mm × 100 mm，1.7 μm）分离，以含0.1%甲酸的乙酸铵（20 mmol/L）水溶液-乙腈体系作为流动相进行梯度洗脱，加热电喷雾离子源正负离子模式，一级全扫描/数据依赖二级扫描（Full MS/dd-MS2）监测模式检测，基质匹配标准曲线外标法定量。结果表明，30种激素在0.5～100 ng/mL浓度范围内线性关系良好，相关系数（r）均大于0.9950；检出限介于0.2～1.0 μg/kg之间，定量限介于0.5～2.0 μg/kg之间；4种不同鱼肉（多宝鱼、鳜鱼、乌鱼、草鱼）在3个添加水平下，回收率为69.7%～103.2%，相对标准偏差为2.3%～9.4%，该方法高效快捷、准确可靠，适用于鱼肉中蛋白同化激素及糖皮质激素的多目标筛查和定量分析。

关键词: 超高效液相色谱-四级杆/静电场轨道阱高分辨质谱, 鱼肉, 蛋白同化激素, 糖皮质激素, 多目标快速筛查

Abstract: A method for rapid screening and identification of 30 protein assimilation hormones and glucocorticoids in fish was established based on UHPLC-Q/Orbitrap high-resolution mass spectrometry. The fish samples were extracted with 80% acetonitrile aqueous solution (containing 0.2% formic acid), centrifuged, purified on Oasis PRiME HLB solid phase extraction column, and redissolved with nitrogen blow. Using Waters Acquity BEH C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column separation, with containing 0.1% formic acid ammonium acetate (20 mmol/L) aqueous solution - gradient elution system of acetonitrile as mobile phase, the positive and negative ions electrospray ion source heating mode, primary Full scan/data dependent on secondary scanning (Full MS/dd-MS2) monitoring pattern detection, matrix matching quantitative standard curve external standard method. The results showed that the linear relationship of the 30 hormones was good in the concentration range of 0.5-100 ng/mL, and the correlation coefficients (r) were all greater than 0.9950. The limits of detection were between 0.2 and 1.0 μg/kg, and the limits of quantification were between 0.5 and 2.0 μg/kg. The recoveries were 69.7%-103.2% and the relative standard deviations were 2.3%-9.4% at three supplemental levels for four different fish (turbalfish, mandarinfish, mullet and grass carp). The method is efficient, accurate and reliable, and is suitable for the rapid multi-objective screening and quantitative analysis of protein assimilation hormones and glucocorticoids in fish.

Key words: UPLC-Q/Orbitrap HRMS, fish, protein assimilation hormone, glucocorticoid, Multi-target rapid screening

中图分类号:

TS207.3

郭添荣吴文林张崟万渝平陈代伟叶梅黄霞张龙翼. 基于UPLC-Q/Orbitrap高分辨质谱多目标快速筛查鱼肉中30种蛋白同化激素及糖皮质激素[J]. 食品科学, 0, (): 0-0.

Wen-Lin WU Yin Zhang. Multi-objective rapid screening of 30 protein assimilation hormones and glucocorticoids in fish based on UPLC-Q/Orbitrap high resolution mass spectrometry[J]. FOOD SCIENCE, 0, (): 0-0.

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