摘要
目的:建立超高效液相色谱—串联质谱(UPLC-MS/MS)检测蜂蜜中苦参碱与氧化苦参碱的分析方法。方法:采用液液萃取前处理技术,蜂蜜样品经水溶解后加入无水硫酸钠,用碱性乙腈萃取,以乙腈和0.1%甲酸—5 mmol/L乙酸铵缓冲液为流动相,用Inspire HILIC色谱柱分离,采用电喷雾正离子扫描,多反应监测(MRM)模式测定,外标法定量。结果:在1~100 ng/mL质量浓度范围内,苦参碱与氧化苦参碱线性关系良好,相关系数R;≥0.998。苦参碱和氧化苦参碱的检出限为0.1μg/kg,定量限为0.3μg/kg。在1,10,100μg/kg加标水平下,苦参碱和氧化苦参碱的平均回收率分别为90.9%~95.1%和80.9%~84.3%,相对标准偏差均<10%(n=6)。将该方法应用至45种市售蜂蜜检测中发现,洋槐蜂蜜中苦参碱和氧化苦参碱的检出率和含量相对较高。结论:该方法准确、快速、灵敏度好,适用于大批量样品的测定,可成为蜂蜜中苦参碱和氧化苦参碱残留的常规检测技术。
Objective:This study aimed to establish a new method for the determination of matrine and oxymatrine in honey by UPLC-MS/MS.Methods:The honey was dissolved in water,and the liquid-liquid extraction pretreatment technology was adopted.The extraction was achieved using ammonia-acetonitrile,with the addition of sodium sulfate to induce a salting out effect.Chromatographic separation was achieved on Inspire HILIC column in the mobile phase composition of acetonitrile and 0.1%formic acid-5 mmol/L ammonium acetate buffer.Mass Spectrometry was carried out under the multiple reaction monitoring(MRM)mode with positive electrospray ionization(ESI+)and external standard method for quantitative analysis.Results:The linear relationship between matrine and oxymatrine was observed in the range of 1~100 ng/mL,with correlation coefficients higher than 0.998.The detection limit and quantitative limit of matrine and oxymatrine in honeywere 0.1μg/kg and 0.3μg/kg,respectively.The average recoveries of matrine and oxymatrine were 90.9%~95.1%and 80.9%~84.3%,respectively,at the spiked levels of 1,10 and 100μg/kg,with the relative standard deviations(RSDS)<10%(n=6).The validated method was then successfully applied to the determination of matrine and oxymatrine in 45 commercially available honey,and the results showed that the detection probability and content of matrine and oxymatrine in acacia honey were relatively high.Conclusion:The established method is accurate,rapid,and sensitive,Moreover,a simultaneous preparation of multiple sample extracts is available,and it can used for the routine determination of matrine and oxymatrine in honey.
作者
荆辉华
向俊
蒋登辉
冯燕英
王云昊
王亮亮
JING Hui-hua;XIANG Jun;JIANG Deng-hui;FENG Yan-ying;WANG Yun-hao;WANG Liang-liang(Hunan Provincial Institute of Product and Goods Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha,Hunan 410117,China;Central South University,School of Chemistry and Chemical Engineering,Changsha,Hunan 410083,China;Hunan Provincial Key Laboratory of Flexible Electronic Materials Genome Engineering,School of Physics and Electronic Sciences,Changsha University of Science and Technology,Changsha,Hunan 410114,China)
出处
《食品与机械》
北大核心
2022年第7期57-62,132,共7页
Food and Machinery
基金
湖南创新型省份建设专项重点研发项目(编号:2020SK2128)
湖南省自然科学联合基金项目(编号:2022JJ90004)。
关键词
苦参碱
氧化苦参碱
液液萃取
超高效液相色谱—串联质谱法
蜂蜜
matrine
oxymatrine
liquid-liquid extraction
ultra performance liquid chromatography-mass spectrometry(UPLC-MS/MS)
honey
