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作 者:李玮 艾连峰 马育松 陈瑞春 郭春海 LI Wei;AI Lianfeng;MA Yusong;CHEN Ruichun;GUO Chunhai(Shijiazhuang Customs Thchnology Center,Shijiazhuang 050051)
机构地区:[1]石家庄海关技术中心
出 处:《分析科学学报》2020年第1期75-80,共6页Journal of Analytical Science
基 金:国家质检总局科技计划(No.2015IK100);河北省科技厅项目(No.19226614D)
摘 要:建立了一种超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)测定辣椒中多种禁用着色剂的方法。样品采用乙腈和正己烷提取,QuEChERS法净化,利用UPLC法分离,在电喷雾正离子及TOF-MS触发TOF-MS/MS的模式下检测,以保留时间、一级离子质量准确度、一级离子同位素分布、二级碎片与库匹配4种手段确保准确定性分析,以TOF-MS提取离子的峰面积定量。结果表明,23种着色剂在10~500 ng/mL浓度范围内线性关系良好,相关系数为0.9411~0.9989,方法定量限为10~100μg/kg,3个添加水平的回收率为61.82%~103.25%,相对标准偏差(n=8)为2.08%~10.56%。该方法具有快速、灵敏、准确和高通量等优点,可应用于实际辣椒样品中多种禁用着色剂的日常检测。A method for determination of several prohibited dyes in chilli by ultra-high performance liquid chromatography coupled with triple quadrupole-time of flight-mass spectrometry(UHPLC-Q-TOF-MS)has been established.The sample was extracted by acetonitrile and n-hexane and cleaned-up with QuEChERS.The samples were detected by the chromatographic system,which were monitored in positive(ESI+)and the TOF-MS-IDA-MS/MS mode.The qualitative analysis of 23 prohibited dyes were confirmed by synergistic effect of retention time,mass accuracy of precursor,isotope distribution of the precursor,and library search.The analytes were quantified by peak areas of the TOF-MS extracted ions.The results showed that the prohibited dyes presented good linearity in the concentration of 10-500 ng/mL with the correlation coefficients ranging from 0.9411 to 0.9989,appropriate recoveries ranging from 61.82%to 103.25% at three spiked levels,and satisfactory RSD(n=8)of 2.08%-10.56%.It was a simple,quick and accurate analytical method for the detection of prohibited dyes in chilli.
关 键 词:超高效液相色谱-四极杆-飞行时间质谱法 高分辨质谱 辣椒 筛查
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