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

Multi-objective Rapid Screening of 30 Protein Assimilation Hormones and Glucocorticoids in Fish by Ultra-high Performance Liquid Chromatography Coupled to Quadrupole/Orbitrap High-Resolution Mass Spectrometry

作　　者：郭添荣 吴文林 张崟[4] 万渝平 叶梅 陈代伟 黄霞 张龙翼 GUO Tianrong;WU Wenlin;ZHANG Yin;WAN Yuping;YE Mei;CHEN Daiwei;HUANG Xia;ZHANG Longyi(Chengdu Institute of Food Inspection,Chengdu 611130,China;Chengdu Institute of Biology,Chinese Academy of Sciences,Chengdu 610041,China;University of Chinese Academy of Sciences,Beijing 100049,China;Key Laboratory of Meat Processing of Sichuan,Chengdu University,Chengdu 610106,China)

机构地区：[1]成都市食品检验研究院,四川成都611130 [2]中国科学院成都生物研究所,四川成都610041 [3]中国科学院大学,北京100049 [4]成都大学肉类加工四川省重点实验室,四川成都610106

出　　处：《食品科学》2022年第4期321-330,共10页Food Science

基　　金：国家市场监督管理总局技术保障专项(2021YJ009);国家现代农业产业技术体系四川创新团队项目(sccxtd-2021-15);四川省科技计划应用基础研究项目(21YYJC0962);成都市技术创新研发项目(2021-YF05-00811-SN)。

摘　　要：建立基于超高效液相色谱-四极杆/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,1.7μm)分离,以含0.1%甲酸的乙酸铵(20 mmol/L)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质量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0.2~1.0μg/kg之间,定量限介于0.5~2.0μg/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。A method for rapid screening and identification of 30 protein assimilation hormones and glucocorticoids in fish was established using ultra-high performance liquid chromatography coupled to quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q/Orbitrap HRMS). The samples were extracted with 80% acetonitrile aqueous solution(containing 0.2% formic acid), centrifuged, purified by solid phase extraction(SPE) on Oasis PRiME HLB column, and dried with nitrogen blow. The residue was re-dissolved. The chromatographic separation was performed on a Waters Acquity BEH C18(2.1 mm × 100 mm, 1.7 μm) column through gradient elution using a mobile phase consisting of 20 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid(A) and acetonitrile(B). The target analytes were detected in the positive and negative ion mode using a heated electrospray ionization(HESI) source through primary full scan/datadependent secondary scan(full MS/dd-MS2) monitoring, and quantitated by matrix-matched external standard method. The results showed that good linearity was observed for the 30 hormones in the concentration range of 0.5–100 ng/mL with correlation coefficients(r) greater than 0.995 0. 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% with relative standard deviations(RSDs)of 2.3%–9.4% at three spiked levels for four different fishes(turbot, mandarin fish, mullet and grass carp). The proposed 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.

关 键 词：超高效液相色谱-四极杆/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 

分 类 号：TS207.3[轻工技术与工程—食品科学]