酸水解结合液相色谱串联质谱法定量检测水产品中总磷酸盐
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1普陀区疾病预防控制中心,浙江 舟山 316100;2舟山市疾病预防控制中心(舟山市卫生 监督所),浙江 舟山 316021

作者简介:

邱凤梅 女 主管技师 研究方向为食品和水质理化检验 E-mail: qiufengmei123@163.com

通讯作者:

方力 男 助理研究员 研究方向为食品和水质理化检验 E-mail: fangli123@126.com

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R155

基金项目:

普陀区公益类科技项目(2025GY07)


Quantification of total phosphate in aquatic products using acid hydrolysis combined with liquid chromatography-tandem mass spectrometry
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1Putuo District Center for Disease Control and Prevention, Zhejiang Zhoushan 316100, China;2Zhoushan City Center for Disease Control and Prevention (Zhoushan Health Supervision Institution), Zhejiang Zhoushan 316021, China

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    摘要:

    目的 旨在建立酸水解结合液相色谱串联质谱法测定水产品中总磷酸盐(以磷酸根计)含量的新方法。方法 样品经提取后用硝酸高温水解,将提取液中焦磷酸盐(P2O74-)、三偏磷酸盐[(PO333-]、三聚磷酸盐(P3O105-)、六偏磷酸盐(P6O186-)等多聚磷酸盐水解转化为正磷酸盐(PO43-),然后注入液相色谱串联质谱仪,电喷雾离子化,选择反应监测模式检测,内标法定量。本研究对检测方法的色谱质谱条件、提取条件及酸水解条件进行了优化,并对所建立方法进行了方法学评价。结果 正磷酸盐在0.1~20.0 mg/L浓度范围内线性关系良好,相关系数>0.999,以3倍和10倍基线噪声所对应的浓度为检出限和定量限时,检测方法的检出限、定量限分别可达0.03 g/kg和0.10 g/kg。在1.0、5.0和10.0 g/kg的加标水平下,方法回收率为84.4%~96.6%,日内、日间相对标准偏差均<10.0%。结论 该检测方法前处理步骤简便、抗基质干扰能力强,准确度高,分析速度快,适用于水产品中总磷酸盐含量的测定。

    Abstract:

    Objective A method for the quantification determination of total phosphate (calculated in PO43-) in aquatic products was established by using acid hydrolysis combined with liquid chromatography-tandem triple quadrupole mass spectrometer (LC-MS/MS).Methods The sample were extracted with nitric acid hydrolysis at boiling water bath, that converted polyphosphates, including pyrophosphate (P2O74-), trimetaphosphate [(PO333-] tripolyphosphate (P3O105-), and hexametaphosphate (P6O186-), into orthophosphate (PO43-). The total phosphate (calculated in PO43-) in the resulting solution following extraction was determined by LC-MS/MS operated in selected reaction monitoring (SRM) mode with negative electrospray ionization. Quantitation was performed using the internal standard method. The chromatography, mass spectrometry, acid hydrolysis, and extraction conditions were optimized, and the established method was validated.Results Good linearity was observed for total phosphate in the concentration range of 0.1 mg/L to 20.0 mg/L, with correlation coefficient greater than 0.999. The limits of detection (LOD) and quantitation (LOQ) of orthophosphate in aquatic products were 0.03 g/kg and 0.10 g/kg, respectively, based on signal-to-noise ratio of 3 and 10. Recoveries ranged from 84.4% to 96.6% at spiked levels of 1.0, 5.0, and 10.0 g/kg, with intra-day and inter-day relative standard deviations (RSDs) both below 10.0%.Conclusion The developed method features simple sample preparation, high resistance to matrix interference, good accuracy, and rapid analysis. It is therefore well-suited for determining total phosphate in aquatic products.

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邱凤梅,张舟听,王宇超,王彩芳,方力.酸水解结合液相色谱串联质谱法定量检测水产品中总磷酸盐[J].中国食品卫生杂志,2026,38(2):121-128.

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  • 收稿日期:2025-12-24
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  • 在线发布日期: 2026-06-01
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