摘要
目的建立高效液相色谱串联质谱(HPLC-MS/MS)法测定木耳中米酵菌酸的方法。方法样品经过1%甲酸-19%水-乙腈提取、强阴离子MAX固相萃取小柱净化,洗脱液氮吹至近干,定容,以ACQUITY UPLC HSS T3(1.8μm,2.1 mm×100 mm)为色谱柱分离,0.01%(v/v)甲酸水和乙腈为流动相进行梯度洗脱,电喷雾负离子多离子监测模式检测,利用基质加标曲线定量,建立HPLC-MS/MS方法。结果米酵菌酸串联质谱方法在5μg/L~120μg/L浓度范围线性关系良好,相关系数为0.9992,检出限是1.0μg/kg,回收率在89.2%~95.9%,相对标准偏差(RSD)为1.72%~4.19%。结论本次建立了木耳中米酵菌酸检测的高效液相三重四极杆质谱方法,适用于木耳中米酵菌酸的风险监测。
Objective To determine bongkrekic acid(BKA)in agaric qualitatively and qualitatively by High-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Method Samples were extracted by 1%ammonia water acetonitrile,purified with strong anion solid phase extraction cartridge of MAX;elution liquid was blown to nearly dry by nitrogen,and constant volume.The BKA was separated on an ACQITY UPLC HSS T3 column(1.8μm,2.1 mm×100 mm),and eluted in gradient with 0.01%formic acid-acetonitrile.Ionization mode was electrospray ionization(ESI)with negative mode and multiplereaction monitoring mode(MRM)was used.The BKA was quantitated by external standard of matrix working curve.HPLC-MS/MS method was established.Results Good linear relationship was obtained for BKA HPLC-MS/MS at a range from 5μg/mL to120μg/Ml;the correlation coefficient was 0.9992.The limit of detection was 1.0μg/kg;the recovery was 89.2%to 95.5%;the RSD was 1.72%to 4.19%.Conclusion the HPLC-MS/MS method established to detect BKA in agaricis applicable to the risk monitoring of BKA in agaric.
作者
张洁
王谢
马青青
张欣烨
苏永恒
张榕杰
ZHANG Jie;WANG Xie;MA Qingqing;ZHANG Xinye;SU Yongheng;ZHANG Rongjie(Laboratory Department,Henan Center for Disease Prevention and Control,Zhengzhou,Henan 450016,China)
出处
《河南预防医学杂志》
2021年第7期496-499,共4页
Henan Journal of Preventive Medicine
基金
河南省重点研发和推广专项(科技攻关)项目(212102311074)
河南省医学科技攻关计划(联合共建)项目(LHGJ20190707,LHGJ20190698,LHGJ20190709)
