摘要
建立了食品接触用纸中23种抗菌剂的超高效液相色谱-静电场轨道阱高分辨质谱(UPLC-Orbitrap HRMS)方法。抗菌剂包含4种对羟基苯甲酸酯类和19种氯苯酚类。样品经甲醇超声提取,离心后氮吹浓缩定容,0.22μm滤膜过滤后进行上机测定。采用色谱柱Waters Atlantis T3(150 mm×2.1 mm,3μm)进行分离,以甲醇-5 mmol/L乙酸铵(含0.4%乙酸)作为流动相梯度洗脱。采用电喷雾负离子(ESI-)模式电离、高分辨质谱的Full MS/dd-MS2扫描模式采集,保留时间及二级子离子质谱图双重定性,以提取离子所得色谱峰面积进行定量。4种对羟基苯甲酸酯类和19种氯苯酚类抗菌剂的定量下限分别为0.05μg/kg和0.05 mg/kg,在0.05~5.0 ng/mL或0.05~5.0μg/mL范围内线性关系良好,相关系数均大于0.997。空白基质样品在3个不同浓度水平的平均加标回收率为81.7%~119%,相对标准偏差为2.0%~8.8%。该方法简单、便捷,可用于食品接触用纸中多种有机抗菌剂的筛查和确证。
An ultra-high performance liquid chromatography-orbitrap high resolution mass spectrometric(UPLC-Orbitrap HRMS)method was established for the determination of 23 organic antibacterial agents,including 4 parabens and 19 chlorophenols in food contact paper products.The samples were ultrasonically extracted with methanol as extraction solvent,then centrifuged,concentrated and fixed volume by nitrogen blowing,filtered by 0.22μm membrane,and finally analyzed by UPLC-Orbitrap HRMS.The separation was performed on a Waters Atlantis T3(150 mm×2.1mm,3μm)by gradient elution,using methanol-5 mmol/L ammonium acetate containing 0.4% acetic acid as mobile phase.Electrospray ionization(ESI-)mode was used for ionization,and full MS/dd-MS2scanning mode for MS.Retention time and secondary subion MS spectrum were used for qualitative analysis,and chromatography peak area of extracted ions was quantified.The limits of quantitation for parabens and chlorophenols were 0.05μg/kg and 0.05 mg/kg,respectively,and the linear relationships were good in the ranges of 0.05-5.0 ng/mL and 0.05-5.0μg/mL,respectively,with correlation coefficients greater than 0.997.The average recoveries for blank matrix samples at three spiked concentrations ranged from 81.7% to 119%,with relative standard deviations of 2.0%-8.8%.The method is convenient and efficient,and could be used for screening and confirmation of organic antibacterial agents in food contact paper.
作者
刘益锋
邱嘉兴
张朋杰
孙克强
张宪臣
赵珍玉
梁润梅
LIU Yi-feng;QIU Jia-xing;ZHANG Peng-jie;SUN Ke-qiang;ZHANG Xian-chen;ZHAO Zhen-yu;LIANG Run-mei(Zhongshan Customs Technology Center,Zhongshan 528400,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2022年第10期1548-1552,共5页
Journal of Instrumental Analysis
基金
拱北海关科技计划项目(2021GK019)。
