藻类保健品中β-N-甲氨基-L-丙氨酸(BMAA)及其同分异构体的检测方法及污染分析
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1.南华大学公共卫生学院;2.深圳市疾病预防控制中心

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国际原子能机构合作研究(CRP_D52044_24959);深圳市医学重点学科建设经费(SZXK066)


The determination of β-N- methylamino -L- alanine(BMAA) and its isomers in algal health products
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Affiliation:

1.ShenZhen Center for Disease Control and Prevention;2.School of Public Health, University of South China

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IAEA Research Contract(CRP_D52044_24959);Shenzhen Key Medical Discipline Construction Fund(SZXK066)

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    摘要:

    目的 建立了藻类保健品中BMAA类毒素基于AQC衍生的液质联用方法,了解当前国内藻类保健品中BMAA类毒素的污染水平。 方法 样品经酸水解、氮气浓缩、AQC衍生后采用超高效液相色谱串联质谱分析,2种同位素内标法定量。 结果 在线性范围0.25 ~ 100 μg/L内,3种BMAA类毒素的相关系数均在0.998以上;当取样15 mg,定容至20.0 mL时,藻类保健品中BMAA、AEG和DAB的检出限分别为133、133和200 μg/kg,定量限分别为443、443和667 μg/kg;回收率在86% ~ 126%之间,相对标准偏差为1.1% ~ 14%。国产藻类保健品中DAB的检出率 (86%) 最高,其次为AEG (23%) 和BMAA (14%);在检出的样品中DAB、AEG和BMAA浓度范围依次为385 ~ 2305 μg/kg、250 ~ 518 μg/kg和472 ~ 698 μg/kg。 结论 本研究建立的AQC衍生-液质联用法操作时间短、准确性高,检测的国产藻类保健品中BMAA类毒素的污染水平较高,应引起重视。

    Abstract:

    ABSTRACT: Objective To establish the liquid chromatography-mass spectrometry method based on AQC derivation for BMAA and its isomers in algal health products, and investigate the pollution levels of algal health products from China. Methods The samples were treated by acid hydrolysis, nitrogen concentration and AQC derivatization, and then analyzed by ultra-performance liquid chromatography-tandem mass spectrometry, quantified by internal standard methods of two commercial isotope standards. Results In the linear range of 0.25 ~ 100 μg/L, the correlation coefficients of BMAA toxions were all above 0.998. When the samples were 15 mg and the volume were 20.0 mL, the detection limits of BMAA, AEG and DAB were 133, 133 and 200 μg/kg, respectively. And the quantitative limits were 443, 443 and 667 μg/kg, respectively. The recoveries were between 86% ~ 126%, with the relative standard deviations (n=6) between 1.1% ~ 14%.The detection rate for DAB was the highest in all samples (86%), followed by AEG (23%) and BMAA (14%). The concentrations of DAB, AEG and BMAA in the detectable samples were between 385 ~ 2305 μg/kg, 250 ~ 518 μg/kg and 472 ~ 698 μg/kg, respectively. Conclusion The established method based on AQC derivation LC-MS/MS method is more efficient and accurate. The levels of BMAA toxins in domestic algae health products were relatively high, it should be paid more attention and to strengthen the supervision.

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  • 收稿日期:2024-01-30
  • 最后修改日期:2024-03-24
  • 录用日期:2024-04-08
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