分散固相萃取-高效液相色谱-串联质谱法测定蜂蜜中生物碱  

Determination of Alkaloids in Honey by Dispersive Solid Phase Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭伟华[1] 周金慧[1] 黄京平[1] 王鹏[1] 李熠[1] 

机构地区：[1]中国农业科学院蜜蜂研究所,农业部蜂产品质量安全风险评估实验室,农业部蜂产品质量监督检验测试中心,北京100093

出　　处：《分析化学》2014年第10期1453-1458,共6页Chinese Journal of Analytical Chemistry

基　　金：中国农业科学院基本科研业务费项目(No.2013ZL032)资助~~

摘　　要：建立了分散固相萃取-高效液相色谱-串联质谱法（ QuEChERS-HPLC-MS/MS）同时测定蜂蜜中吡咯里西啶生物碱（倒千里光、千里光菲林、千里光宁、克氏千里光宁）和异喹啉类生物碱（小檗碱、荷叶碱）的方法。蜂蜜样品经乙腈提取,乙二胺-N-丙基硅烷（ PSA）吸附剂净化,HPLC-MS/MS测定。采用Agilent Poroshell 120 SB-C18色谱柱（100 mm2×2.7μm）分离。以0.1%甲酸溶液和乙腈为流动相进行梯度洗脱,电喷雾正离子（ESI＋）模式电离,多反应监测模式（MRM）下进行测定,外标法定量。结果表明,在0.1～100μg/L范围内,6种生物碱的相关系数均大于0.99；在1～100μg/kg的添加水平下,所有生物碱回收率均在70%～110%之间；6种生物碱日内精密度小于15%,日间精密度小于20%；方法检出限和定量限分别为0.3和1.0μg/kg。本方法可用于蜂蜜中吡咯里西啶生物碱和异喹啉类生物碱的同时定性和定量分析。A method was developed for simultaneous determination of pyrrolizidine alkaloids and isoquinoline alkaloids in honey by dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry （ QuEChERS-HPLC-MS/MS） . The honey samples were extracted with acetonitrile solution and cleaned up with PSA absorbent. Agilent Poroshell 120 SB-C18 chromatographic column was used to separate alkaloids with high sensitivity and satisfactory resolution. The identification and quantification were achieved by using electrospray ionization in positive ion mode （ ESI＋） with multiple reaction monitoring （MRM）. Matrix-matched calibration curves with good correlation coefficients （R2〉0. 99） were obtained in the concentration range of 0. 1-100 μg/L. The recoveries of the spiked samples at 1-100 μg/kg were in the range of 70% to 110% with the RSD of intra-day and inter-day lower than 15% and 20%, respectively. The limits of detection （ LOD） and limits of quantification （ LOQ） for all alkaloids were 0. 3 and 1. 0 μg/kg, respectively. This method was successfully applied to the simultaneous determination of pyrrolizidine alkaloids and isoquinoline alkaloids for quantification and confirmation in honey samples.

关 键 词：分散固相萃取 高效液相色谱-串联质谱法 吡咯里西啶生物碱 异喹啉类生物碱 蜂蜜 

分 类 号：O657.63[理学—分析化学] S896.1[理学—化学]