干旱区生态环境知识资源中心(Arid): 全自动固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中硝基呋喃类代谢物

Arid

	全自动固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中硝基呋喃类代谢物
其他题名	Determination of Nitrofuran Metabolites in Honey By Auto-Solid Phase Extraction-Ultra-high Performance Liquid Chromatography-Tandem Mss Spectrometry
	毛思浩; 刘柱; 梁晶晶; 陈万勤; 徐潇颖; 赵超群; 王峰
来源期刊	分析科学学报
ISSN	1006-6144
出版年	2020
卷号	36 期号:4 页码:572-578
中文摘要	建立了全自动固相萃取,结合超高效液相色谱-串联质谱法同时测定蜂蜜中5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)、3-氨基-2-唑烷基酮(AO Z)、1-氨基乙内酰脲(AHD)和氨基脲(SEM)4种硝基呋喃代谢物的分析方法。样品经0.2mol/L HCl提取,同时与2-硝基苯甲醛进行衍生化反应,调节衍生液pH值至7.2~7.4,选择Oasis HLB作为固相萃取柱,采用全自动固相萃取仪进行富集净化。采用Agilent ZORBAX SB-C_(18)色谱柱分离,以乙腈和5mmol/L NH4Ac溶液(含0.1%甲酸)为流动相梯度洗脱;质谱以电喷雾离子源电离,正离子多反应监测(MRM)模式检测,同位素内标法定量。结果表明:4种硝基呋喃类代谢物在1.0~20mug/L范围内线性关系良好,相关系数均大于0.999;方法检出限为0.04~0.08mug/kg;在0.25、1. 25、2.5mug/kg不同水平的加标试验,平均回收率在100.6%~102.3%之间,相对标准偏差(RSD,n=6)在0.52%~2.0%之间。该方法前处理处理过程便捷、高效、稳定,在回收率以及重复性方面优于外标定量法和国家标准(GB/T 18932.24-2005)法,更适用于蜂蜜中硝基呋喃代谢物含量的检测。
英文摘要	An auto-solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(ASPE-UHPLC-MS/MS)method was established for the simultaneous determination of 5-morpholino- 3-amino-2-oxazolidone(AMOZ),3-amino-2-oxazolidinone(AOZ),1-amino-hydanto in(AHD),semicarbazide(SEM)in honey.The samples were extracted with 0.2mol/L hydrochloric acid solution,and derivatized with 2-nitrobenzaldehyde simultaneously.The pH of derivatization was controlled at 7.2-7.4.Auto-solid phase extraction was applied to enrichment and purification with an Oasis HLB column.An Agilent ZORBAX SB-C_(18)column was used for separation with acetonitrile-5mmol/L ammonium acetate solution(containing 0.1%formic acid)as mobile phase.The samples were detected under positive ions multiple reaction monitoring(MRM)mode and quantitatived by isotope internal standard method.The results showed that the metabolites of four nitrofuran metabolites had good linearity in the range of 1.0-20mug/L,and the correlation coefficients were better than 0.999.The limits of detection(LODs)of four targets were in the range of 0.04-0.08mug/kg.The average recoveries of all the compounds at three spiked levels of 0.25,1.25,2.5mug/kg ranged from 100.6%to 102.3% with RSDs(n=6)of 0.52%-2.0 %.The pretreatment process of the method is convenient,efficient and stable.The method is better than external standard quantitation and GB/T 18932.24-2005 method in recovery and repeatability,and is more suitable for the detection of nitrofuran metabolites in honey.
中文关键词	蜂蜜 ; 硝基呋喃代谢物 ; 全自动固相萃取 ; 超高效液相色谱-串联质谱
英文关键词	Honey Nitrofuran metabolites Auto-solid phase extraction Ultra-high performance liquid chromatography-tandem mass spectrometry
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6806981
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353429
作者单位	毛思浩, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 刘柱, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 梁晶晶, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 陈万勤, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 徐潇颖, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 赵超群, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 王峰, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国.
推荐引用方式 GB/T 7714	毛思浩,刘柱,梁晶晶,等. 全自动固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中硝基呋喃类代谢物[J],2020,36(4):572-578.
APA	毛思浩.,刘柱.,梁晶晶.,陈万勤.,徐潇颖.,...&王峰.(2020).全自动固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中硝基呋喃类代谢物.分析科学学报,36(4),572-578.
MLA	毛思浩,et al."全自动固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中硝基呋喃类代谢物".分析科学学报 36.4(2020):572-578.