Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Fishery Quality Supervision and Testing Center of Ministry of Agriculture and Rural Affairs, Fishery Products Quality Safety Risk Assessment Laboratory (Wuhan) of Ministry of Agriculture and Rural Affairs, Wuhan 430223, China.
Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Fishery Quality Supervision and Testing Center of Ministry of Agriculture and Rural Affairs, Fishery Products Quality Safety Risk Assessment Laboratory (Wuhan) of Ministry of Agriculture and Rural Affairs, Wuhan 430223, China; Key Laboratory of Control of Quality and Safety for Aquatic Products of Ministry of Agriculture and Rural Affairs, Beijing 100141, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 May 1;1171:122622. doi: 10.1016/j.jchromb.2021.122622. Epub 2021 Mar 10.
A widely applicable method was established and validated for the qualitative and quantitative analysis of twenty-six triazine herbicides in multiple fish and seafood using ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). New convenient sample preparation approach based on modified QuEChERs was proposed by adding EMR-lipid to the traditional QuEChERS purification agents. Good separation was obtained after gradient elution through a C column. Target compounds were detected with electrospray ionization in positive ion mode and quantified in selective reaction monitoring (SRM) mode. Under this effective method, satisfactory results of linearity, sensitivity, accuracy, precision and matrix effect were achieved. Good linearities of the calibration curves yielded the correlation coefficients higher than 0.996 for all herbicides. The LOQs of 26 triazine herbicides ranged from 0.5 to 1.0 ng g. Good accuracy and precision were shown with the recoveries at the concentration of 1.0, 5.0 and 20.0 ng g from 70.1% to 111.7% and the precisions of intra- and inter-day less than 12%. The matrix effects (-21.8-27.6%) were almost negligible. Finally the method was applied to the analysis of 72 crayfish samples from breeding bases of Hubei and Hunan provinces (China).
建立并验证了一种超高效液相色谱串联质谱法(UHPLC-MS/MS),可用于定性和定量分析多种鱼类和海鲜中的二十六种三嗪类除草剂。通过在传统 QuEChERS 净化剂中添加 EMR-脂质,提出了一种新的简便的样品前处理方法。在 C 柱上进行梯度洗脱后,可获得良好的分离效果。目标化合物采用电喷雾电离正离子模式检测,选择性反应监测(SRM)模式定量。在这种有效的方法下,线性、灵敏度、准确度、精密度和基质效应均取得了令人满意的结果。所有除草剂的校准曲线均具有良好的线性,相关系数均高于 0.996。26 种三嗪类除草剂的 LOQs 范围为 0.5-1.0 ng/g。在 1.0、5.0 和 20.0 ng/g 浓度下的回收率为 70.1%-111.7%,日内和日间精密度均小于 12%,表明准确度和精密度良好。基质效应(-21.8%-27.6%)几乎可以忽略不计。最后,该方法应用于分析来自湖北和湖南养殖基地的 72 只小龙虾样品。