中国食品添加剂2024，Vol.35Issue(12)：177-185,9.DOI:10.19804/j.issn1006-2513.2024.12.022
液相色谱串联质谱法检测草鱼中地西泮优化实验研究
Determination of diazepam residues in grass carp using liquid chromatography tandem mass spectrometry
摘要
Abstract
In order to establish a Liquid Chromatography-Tandem Mass Spectrometry(LC-MS/MS)method for the detection of diazepam residues in aquatic products with simple pretreatment operation and high recovery rate,taking grass carp products samples as a case study,the samples were extracted by 3%ammonia-ethyl acetate,followed by parallel rotary evaporation for concentration,purified using neutral alumina solid phase extraction column(Alumina N SPE).Quantitative analysis was performed using external standard method.The results showed that the method was easy to operate,with the recovery rates of the method in grass carp samples ranging from 82.0%to 93.6%,and the relative standard deviation was less than 5%.When the diazepam content in grass carp samples was 2.34 μg·kg-1,its expanded uncertainty was 0.16 μg·kg-1(k=2).In practical application,the recovery rate remained stable at over 80%,with an intra-batch relative standard deviation was less than 5%,and the inter-batch relative standard deviation was less than 10%,so the method was suitable for the detection of diazepam in various aquatic products,including carp,crucian carp,silver carp,bighead carp and grass carp.关键词
地西泮/中性氧化铝固相萃取柱/液相色谱-串联质谱法/不确定度Key words
diazepam/neutral alumina solid phase extraction column/liquid chromatography-tandem mass spectrometry/uncertainty分类
轻工纺织引用本文复制引用
李娜,王进福,王爱英,杨艳艳,刘红彩,陈爱景,王超,孙栋..液相色谱串联质谱法检测草鱼中地西泮优化实验研究[J].中国食品添加剂,2024,35(12):177-185,9.基金项目
山东省自然科学基金项目(ZR2022MC170) （ZR2022MC170）
