液-质联用法测定双香豆素类化合物在水中的含量及对斑马鱼的急性毒性  

Determination of the contents of biscoumarin compounds in water and their acute toxicity to zebrafish by LC-MS

作　　者：范继文 李维政 梁赫 赵娜娜[1] 王天琴 张乐 路伟[1] FAN Ji-wen;LI Wei-zheng;LIANG He;ZHAO Na-na;WANG Tian-qin;ZHANG Le;LU Wei(Engineering Research Centre of Cotton,Ministry of Education,College of Agriculture,Xinjiang Agricultural University,Urumqi 830052,China;Guorino Drug Safety Evaluation Research Co.,Ltd.,Xi'an 710000,China)

机构地区：[1]新疆农业大学农学院棉花教育部工程研究中心,乌鲁木齐830052 [2]国睿一诺药物安全评价研究有限公司,西安710000

出　　处：《农药》2022年第11期827-832,共6页Agrochemicals

基　　金：国家重点研发计划项目(2017YFD0201903);天山创新团队计划项目(2020D14001);新疆农科院科技创新重点培育专项(xjkcpy-2020004)。

摘　　要：[目的]建立4种双香豆素类化合物(biscoumarin,BCM)的液-质分析方法;评价4种BCM对斑马鱼的安全性。[方法]采用液-质联用仪测定水中4种双香豆素类化合物的含量,确定其暴露浓度;采用半静态法测定双香豆素类天然产物衍生物对斑马鱼的急性毒性。[结果]BCM4、BCM7、BCM8、BCM12标样的峰面积(y)与质量浓度(x)呈线性关系,决定系数R^(2)均>0.9900,最低检测浓度LOQ为0.2 mg/L,BCM4、BCM8、BCM12高、低质量浓度的添加剂量分别为80.0、20.0 mg/L,BCM7高、低质量浓度的添加剂量分别为8.0、2.0 mg/L,4种BCM的添加回收率介于95.20%~113.60%之间。BCM4、BCM7、BCM8、BCM12对斑马鱼急性毒性96 h的LC分别为33.75、13.31、41.19、48.42 mg/L。[结论]使用高效液-质联用仪测定BCM4、BCM7、BCM8、BCM12在水中的含量所采用的检测方法精密度和准确度良好,4种BCM对斑马鱼的急性毒性为低毒。[Aims] This study aims to establish a LC-MS analysis method for evaluation of the safety of 4 biscoumarin compounds BCM on zebrafish. [Methods] The contents of four biscoumarin compounds in water were texted by LC-MS and their exposure concentrations were determined. The acute toxicity of biscoumarin derivatives to zebrafish was determined by semi-static method. [Results] The peak area(y) of BCM4, BCM7, BCM8 and BCM12 samples showed a linear relationship with the concentration(x), and the determination coefficients R^(2)were all >0.9900, the lowest detection concentration LOQ was 0.2 mg/L, the high and low concentrations of BCM4, BCM8, BCM12 were80.0, 20.0 mg/L, the high and low concentrations of BCM7 were 8.0, 2.0 mg/L, respectively. The recoveries of the four kinds of BCM ranged from 95.20% to 113.60%. The LCof acute toxicity of BCM4, BCM7, BCM8 and BCM12 to zebrafish at 96 h were 33.75, 13.31, 41.19 and 48.42 mg/L, respectively. [Conclusions] The determination method of BCM4, BCM7, BCM8 and BCM12 in water by LC-MS was precise and accurate, and the acute toxicity of four kinds of BCM to zebrafish was low.

关 键 词：双香豆素类化合物 斑马鱼 急性毒性 液-质联用仪 

分 类 号：TQ450.2[化学工程—农药化工]