摘要
建立了水产品中6种丁香酚类化合物的二甲亚砜(DMSO)辅助浓缩-气相色谱-质谱联用仪(GC-MS)测定方法。试样加入无水硫酸钠后,以乙腈为提取溶剂,乙腈饱和的正己烷脱脂,乙腈层加入二甲亚砜(DMSO)辅助氮吹浓缩至近干;采用DB-1701色谱柱进行分离,并用质谱进行检测。6种化合物在20~1000μg/L内呈良好的线性关系(相关系数大于0.999);在四种基质中的加标水平分别为0.02、0.04、0.10 mg/kg时,6种化合物平均加标回收率为64.8%~110.9%,相对标准偏差均不大于15%(n=6);方法定量限为0.02 mg/kg。该方法灵敏、准确度高、快速、线性范围宽、选择性好、前处理简单,并解决了目前文献方法中仅直接氮吹浓缩对回收率影响很大的关键问题,适用于水产品中丁香酚类化合物的准确定性定量检测,可用于水产品中该类麻醉剂的摸底监测。
An analytical method was developed for determination of six kinds of eugenol drug residues in aquatic products at the same time by using DMSO assisted concentration and GC-MS.Sample was ultrasonic extracted by acetonitrile after adding anhydrous sodium sulfate,degreased using acetonitrile saturated n-hexane.The acetonitrile layer was added with DMSO for nitrogen blowing to nearly dry and determined by GC-MS using DB-1701.Six analytes had good relationships in concentration range of 20~1000μg/L,the correlation coefficients were not less than 0.999,and the average recovery rates under the three different concentrations were 64.8%~110.9%(n=6).This method was simple,rapid,with good repeatability,good stability and good accuracy,and reduced analyte losses in nitrogen blowing significantly.The method was suitable for the determination of clove phenol drug residues in aquatic products and qualitative confirmation research.
作者
余晓琴
方科益
邵曼
李澍才
陈小泉
YU Xiao-qin;FANG Ke-yi;SHAO Man;LI Shu-cai;CHEN Xiao-quan(Sichuan Provincial Food and Drug Inspection Institute,Chengdu 610000,China;Technology Center of Ningbo Customs,Ningbo 315000,China)
出处
《食品工业科技》
CAS
北大核心
2020年第17期258-262,268,共6页
Science and Technology of Food Industry
关键词
水产品
丁香酚类
二甲亚砜
气相色谱-质谱联用仪(GC-MS)
aquatic products
clove phenol drug residues
dimethyl sulfoxide
gas chromatography-tandem mass spectrometry(GC-MS)
