超高效液相色谱-三重四极杆串联质谱法测定蜂蜜中吡咯里西啶类生物碱  

Determination of five pyrrolizidine alkaloids in honey by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry

作　　者：程莉[1,2] 王丹[1] 周爽[1] 张加玲[2] 赵云峰[1] 

机构地区：[1]国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室,北京100021 [2]山西医科大学公共卫生学院,太原030001

出　　处：《环境化学》2014年第11期1971-1977,共7页Environmental Chemistry

基　　金："十二五"国家科技支撑计划课题(2012BAK01B01)资助

摘　　要：建立了蜂蜜中5种吡咯里西啶类生物碱的超高效液相色谱-串联质谱测定方法.蜂蜜样品用50%甲醇超声提取,强阳离子交换固相萃取柱净化富集,超高效液相色谱-三重四极杆串联质谱MRM模式检测,外标法定量.以Waters BEH C18(100 mm×2.1 mm,1.7μm)色谱柱分离,以含0.1%甲酸的乙腈和0.1%甲酸水溶液进行梯度洗脱.倒千里光碱、千里光宁、千里光菲啉和野百合碱在0.2—100.0μg·kg-1,克氏千里光宁在1.0—200.0μg·kg-1的浓度范围内各化合物线性关系良好,相关系数r均大于0.999,定量限在0.2—0.8μg·kg-1之间.在3个加标水平下,空白基质蜂蜜中的5种生物碱的平均回收率为82.0%—110.0%之间,相对标准偏差(RSD)小于12.5%.方法准确可靠,适合于蜂蜜中吡咯里西啶类生物碱的测定.An ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry（ UPLC-MS / MS） method for the determination of five pyrrolizidine alkaloids（ retrorsine,senecionine,seneciphylline,crotaline and senkirkine） in honey was established.Samples were extracted with 50% methanol solution and purified with a strong-cation exchange column. Analyte separation was achieved using a Waters BEH C18（ 100 mm × 2. 1 mm,1. 7 μm）clumn with a mobile phase of 0. 1% formic acid in acetonitrile and 0. 1% formic acid in water. The separated compounds were detected in multiple reaction monitoring（ MRM） mode using positive electrospray ionization（ ESI＋）. Retrosine,senecionine,seneciphylline,and crotaline showed a good linearity in the range of 0. 2—100. 0 μg·kg- 1,and senkirkine in the range of 1. 0—200. 0 μg·kg- 1（ r 0. 999）. The limit of quantification of the PAs was 0. 2—0. 8 μg·kg- 1. Recovery rates in blank spiked samples were between 82. 0% —110. 0% and the relative standard deviation was below12. 5%. This method was accurate,sensitive and suitable for the determination of PAs in honey.

关 键 词：吡咯里西啶类生物碱 超高效液相色谱-三重四极杆串联质谱法 蜂蜜 

分 类 号：X836[环境科学与工程—环境工程] O657.63[理学—分析化学]