| 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) |
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| Study on the determination method of semicarbazide existing form in shellfish |
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Xing Li Hong, Sun Wei Hong, Zhu Pan Pan, Sun Xiao Jie, Li Zhao Xin
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Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences
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| 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 |