藻类保健品中β-N-甲氨基-L-丙氨酸及其同分异构体的检测方法及污染分析  

The determination and pollution analysis ofβ-N-methylamino-L-alanine and its isomers in algal health products

作　　者：王琛 袁冠湘 罗青 秦逍云[2] 杨胜园[1] 刘桂华 WANG Chen;YUAN Guanxiang;LUO Qing;QIN Xiaoyun;YANG Shengyuan;LIU Guihua(School of Public Health,University of South China,Hu’nan Hengyang 421001,China;Shenzhen Center for Disease Control and Prevention,Guangdong Shenzhen 518055,China)

机构地区：[1]南华大学公共卫生学院,湖南衡阳421001 [2]深圳市疾病预防控制中心,广东深圳518055

出　　处：《中国食品卫生杂志》2024年第6期672-679,共8页Chinese Journal of Food Hygiene

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

摘　　要：目的建立藻类保健品中β-N-甲氨基-L-丙氨酸(BMAA)类毒素基于6-氨基喹啉基-N-羟基琥珀酰亚氨基甲酸酯(AQC)衍生的液质联用检测方法,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0.25~100μg/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、N-2-氨乙基甘氨酸(AEG)和2,4-二氨基丁酸(DAB)的检出限分别为133、133和200μg/kg,定量限分别为443、443和667μg/kg;回收率在86.7%~126.0%之间,相对标准偏差为1.1%~14.0%。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385~2305μg/kg、250~518μg/kg和472~698μg/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。Objective To investigate the pollution levels of algal health products in China,the liquid chromatographymass spectrometry method based on AQC derivation for BMAA and its isomers in algal health products was established.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 0.25-100μg/L,the correlation coefficients of BMAA toxins 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 200μg/kg,respectively.And the quantitative limits were 443,443 and 667μg/kg,respectively.The recoveries were between 86.7%and 126.0%,with the relative standard deviations between 1.1%and 14.0%.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 385-2305,250-518 and 472-698μg/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.

关 键 词：藻类保健品 β-N-甲氨基-L-丙氨酸(BMAA) 2 4-二氨基丁酸(DAB) N-2-氨乙基甘氨酸(AEG) 

分 类 号：R155[医药卫生—营养与食品卫生学]