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食品研究与开发:2018,39(1):113-117
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LILIC-Q/TOF对乳粉中羟脯氨酸的确证分析
王骏,胡梅,李恒,徐大玮,薛霞,祝建华
(山东省食品药品检验研究院,山东济南250101)
Confirmatory Analysis of Hydroxyproline in Milk Powder by LILIC-Q/TOF
WANG Jun,HU Mei,LI Heng,XU Da-wei,XUE Xia,ZHU Jian-hua
(Shandong Institute for Food and Drug Control,Jinan 250101,Shandong,China)
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投稿时间:2017-03-14    
中文摘要: 建立亲水作用色谱-四极杆飞行时间质谱测定乳粉中羟脯氨酸的确证方法。乳粉样品经盐酸水解后,以HLB固相萃取柱净化,经亲水作用色谱柱分离后,使用超高效液相色谱-四极杆/飞行时间质谱分别进行全扫描和羟脯氨酸的二级质谱扫描分析,以羟脯氨酸的色谱保留时间、母离子和碎片离子的精确质量数对其进行确证分析。方法的检测限优于0.1mg/kg,可满足乳粉中非法添加羟脯氨酸的确证分析要求。
Abstract:A confirmatory analytical method was developed for the determination of hydroxyproline in milk powder using hydrophilic interaction chromatography coupled with quadrupole-time of flight-mass spectrometry(HILIC-Q/TOF).The samples were hydrolyzed with hydrochloric acid,and cleaned up by solid phase extraction,and the protein was precipitated with acetonitrile subsequently.After separated on an Acquity UPLC BEH HILIC column,hydroxyproline was carried out in the full scan and daughter ion scan mode.The hydroxyproline was confirmed by the retention time,accurate mass of parent ion and fragment ions,and the detection limit was better than 0.1mg/kg.The method was suitable for the confirmation of hydroxyproline in milk powder.
文章编号:201801022     中图分类号:    文献标志码:
基金项目:山东省重点研发计划项目(2015GSF120018)
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