摘要
建立了蜂蜜中33种生物碱的高效液相色谱-串联质谱测定方法。样品使用乙腈提取,提取液采用PSA粉末进行净化,选择Agilent ZORBAX Eclipse Plus C18色谱柱(50 mm×3.0 mm,1.8μm)分离,以0.1%甲酸水-甲醇作为流动相进行梯度洗脱,在电喷雾正离子多反应监测模式下,以保留时间和特征离子对信息进行定性和定量分析。结果表明,在0.5~50μg/L浓度范围内,33种生物碱均具有良好的线性关系,方法的检出限(S/N=3)和定量限(S/N=10)分别为0.33~6.7、1.0~20μg/kg。对蜂蜜基质中进行2.0、4.0、20μg/kg 3水平的加标回收试验,经基质匹配标准曲线校正,33种目标生物碱中28种的回收率范围为64.5%~100.2%,相对标准偏差在4.7%~14.6%之间,方法回收率和精密度良好;5种的回收率低,无法满足相关技术要求,只能定性分析。本方法操作简单,灵敏度高,可以快速地对蜂蜜中生物碱进行定性和定量分析。
A novel method for analysis of 33 kinds of toxic alkaloids in honey samples by high performance liquid chromatography-tandem mass spectrometry was developed,employing Agilent column(50 mm×3.0 min,1.8 μm) and 0.1% formic acid-methanol system as the mobile phase.In view of the significant differences in the structure and chemical nature of these alkaloids,samples were directly extracted with acetonitrile.The purification of the alkaloids was carried out on by PSA.The identification and quantification were achieved by using electrospray ionization in positive ion mode with multiple reaction monitoring via the retention time and characteristic ion pair.Under the optimal conditions,the linearity of the calibration curves of all alkaloids was observed over the concentration range of 0.5-50.0 ng/mL with good correlation coefficient R2 > 0.99.The limits of quantification was 1.0-20 μg/kg(S/N=10),and the limit of detection was demonstrated as 0.33-6.7 μg/kg(S/N=3).At spiked levels of 2.0,4.0,20 μg/kg,the average recoveries of alkaloids in spiked samples ranged from 64.5% to 100.2%,with relative standard deviations between 4.7% and 14.6% for 28 alkaloids.The recoveries of 5 kinds alkaloids in the honey was poor,including Ephedrine hydrochloride,Monocrotaline,Sophoridine,Chelerythrinea and Antu.The method could meet the requirement for rapid screening and quantitative analysis of toxic alkaloids in foods,with the advantages of simple operation,low detection limit,high sensitivity and good stability to provide the basis for the safety evaluation.
作者
杜凤君
徐敦明
张志刚
林玉萍
林立毅
赖国银
赵海军
刘舟
王娟
吕美玲
DU Feng-jun;XU Dun-ming;ZHANG Zhi-gang;LIN Yu-ping;LIN Li-yi;LAI Guo-yin;ZHAO Hai-jun;LIU Zhou;WANG Juan;L Mei-ling(Technology Center,Xiamen Customs,Xiamen 361026;Xiamen Medical College,Xiamen 361023;Agilent Technologies(China)Co.Ltd,Beijing 100102)
出处
《分析科学学报》
CAS
CSCD
北大核心
2019年第6期817-823,共7页
Journal of Analytical Science
基金
福建省社会发展引导性(重点)项目(No.2018Y0075)
原国家质检总局科技计划(No.2017IK091)
