| 摘要: |
| 为明确环境新型污染物--氨基脲(semicarbazide,SEM)在贝类体内的存在形态,本文建立了一种SEM在扇贝中形态测定的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)分析方法。扇贝中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%,相对标准偏差均<15%。本方法扇贝中SEM的定量限为1.0 μg/kg,本方法灵敏、准确、操作简便,适用于扇贝中SEM存在形态的测定。 |
| 关键词: 氨基脲 液相色谱-串联质谱法 扇贝 存在形态 |
| DOI：10.11759/hykx20211119001 |
| 分类号:S912 |
| 基金项目:国家自然科学基金项目(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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| Determination method of the semicarbazide existing form in scallop |
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XING Li-hong1,2,3,4, SUN Wei-hong1,2,3,4, ZHU Pan-pan1,2,3,4, SUN Xiao-jie1,2,3,4, LI Zhao-xin1,2,3,4
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1.Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture and Rural Affairs, China;2.Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China;3.Pilot National Laboratory for Marine Science and Technology, Qingdao 266003, China;4.Collaborative Innovation Center of Seafood Deep Processing, Dalian Polytechnic University, Dalian 116034, China
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| Abstract: |
| In order to clarify the existing form of a new environmental pollutant semicarbazide (SEM) in shellfish, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to determine the existing form of the environmental pollutant semicarbazide (SEM) in scallop. The total SEM in scallop was determined as follows: After hydrolysis by hydrochloric acid, the sample was derivatized by 2-nitrobenzaldehyde overnight for 16 hours. Then, SEM was extracted with ethyl acetate, purified by ultrafiltration, and analyzed using LC-MS/MS. The tissue-bound SEM was separately washed with methanol/water (50: 50; v/v), followed by methanol/water (75: 25; v/v), methanol, and water. 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 (electrospray ionization, ESI+) with selected reaction monitoring, identification of the major components of the SEM residue was performed based on the fragment intensities. The calibration curve showed good linearity from 0.5-20 μg/L, with a correlation coefficient over 0.999. The recoveries 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 were less than 15%, and the limit of quantitation for the SEM in scallop tissue was 1.0 μg/kg. The proposed method is sensitive, accurate, and easy to operate, which is suitable for determining the existing form of SEM in scallop. |
| Key words: SEM high-performance liquid chromatography-tandem mass spectrometry scallop existing form |
