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氨基脲在贝类中的形态测定方法研究
邢丽红, 孙伟红, 朱盼盼, 孙晓杰, 李兆新
中国水产科学研究院黄海水产研究所
摘要:
建立一种环境污染物氨基脲(semicarbazide, SEM)在贝类中存在形态的液相色谱-串联质谱(liquidSchromatography-tandem mass spectrometry, LC-MS/MS)测定方法。贝类中SEM总量测定方法为,样品用盐酸水解,以2-硝基苯甲醛为衍生剂衍生,乙酸乙酯提取,超滤离心净化,进LC-MS/MS分析。结合态SEM测定方法为,样品分别采用50%甲醇水溶液、75%甲醇水溶液、甲醇和水洗涤后,按照SEM总量测定方法处理,采用甲醇和2 mmol/L乙酸铵作为流动相进行梯度洗脱,电喷雾离子源正离子(electrosprary ionization, ESI+)选择反应监测模式对SEM进行定性和定量测定。本方法在1~20 μg/L范围内线性关系良好,相关系数大于0.999。SEM在1.00、5.00、10.0 μg/kg添加水平的回收率在84.2%~118%之间,相对标准偏差均<15%。本方法贝类中SEM的定量限为1.0 μg/kg。结论 该方法灵敏、准确,操作简便,适用于贝类中SEM存在形态的测定。
关键词:  氨基脲  液相色谱-串联质谱法  贝类  存在形态
DOI:
分类号:S912
基金项目:国家自然科学(41806148),浙江省近岸水域生物资源开发与保护重点实验室、温州市海洋生物遗传育种重点实验室联合开放基金(J2021003),中国水产科学研究院基本科研业务费(2020TD71)
Study on the determination method of semicarbazide existing form in shellfish
Xing Li Hong, Sun Wei Hong, Zhu Pan Pan, Sun Xiao Jie, Li Zhao Xin
Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences
Abstract:
A liquidSchromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of existing form of environmental pollutant semicarbazide(SEM) in shellfish. The total SEM in shellfish was determined as following: After hydrolyzed by hydrochloric acid, the sample was derivatized by 2-nitrobenzaldehyde overnight with 16 hours. Then SEM was extracted with ethyl acetate and purified by ultrafiltration, and analyzed by LC-MS/MS. The tissue bound SEM was washed with methanol/water (50:50; v/v), followed by methanol/water (75:25; v/v), methanol and water, separately. Then the sample was determined as the method of the total SEM. The SEM residue in the extract was separated on a reversed phase using a gradient elution program of methanol and 2 mmol/L ammonium acetate. Using LC-MS/MS (electrosprary ionization, ESI+) with selected reactions monitoring, identification of the major components of the SEM residue was performed based upon the intensities of fragments. The calibration curve showed a good linearity in a range of 0.5-20 μg/L with the correlation coefficient over 0.999. The recoveries were ranged from 84.2% to 118% for the SEM residues with 3 spiked levels at 1.00, 5.00 and 10.0 μg/kg. The relative standard deviations (RSDs) were less than 15%, and the limit of quantitation (LOQ) for the SEM in the tissue of shellfish was 1.0 μg/kg. The proposed method is sensitive, accurate and easy to operate, which is suitable for the determination of the existing form of SEM in shellfish.
Key words:  SEM  high performance liquid chromatography-tandem mass spectrometry  shellfish  existing form
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