全自动在线固相萃取-液相色谱-高分辨质谱法测定麦卢卡蜂蜜中的特征标志物  

Determination of characteristic compound in manuka honey by automatic on-line solid phase extraction-liquid chromatography-high resolution mass spectrometry

作　　者：沈崇钰[1] 郭思言[2] 丁涛[1] 刘芸[1] 陈磊[1] 费晓庆[1] 张睿[1] 吴斌[1] 沈伟健[1] 陈雷[1] 张峰[3] 冯峰[3] 邓晓军[4] 伊雄海[4] 杨功俊[2] 陈国强 SHEN Chongyu;GUO Siyan;DING Tao;LIU Yun;CHEN Lei;FEI Xiaoqing;ZHANG Rui;WU Bin;SHEN Weijian;CHEN Lei;ZHANG Feng;FENG Feng;DENG Xiaojun;YI Xionghai;YANG Gongjun;CHEN Guoqiang(Animal,Plant and Food Inspection Center,Jiangsu Entry-Exit Inspection and Quarantine Bureau,Nanjing 210001,China;College of Pharmacy,China Pharmaceutical University,Nanjing 211198,China;Chinese Academy of Inspection and Quarantine,Beijing 102600, China;Shanghai Entry-Exit Inspection and Quarantine Bureau,Shanghai 200135,China;Suzhou Entry-Exit Inspection and Quarantine Bureau,Suzhou 215004,China)

机构地区：[1]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001 [2]中国药科大学药学院,江苏南京211198 [3]中国检验检疫科学研究院,北京102600 [4]上海出入境检验检疫局,上海200135 [5]苏州出入境检验检疫局,江苏苏州215004

出　　处：《色谱》2017年第10期1068-1072,共5页Chinese Journal of Chromatography

基　　金：国家重点研发计划(2017YFF0211000);上海长三角科技合作项目(15395810100)~~

摘　　要：建立了全自动在线固相萃取-液相色谱-高分辨质谱(SPE-LC-HRMS)测定麦卢卡蜂蜜中特征标志物3,5-二甲氧基苯甲酸甲酯-4-双葡萄糖糖苷(leptosperin)的方法。以Dikma Diamonsil Plus C_(18)色谱柱(150 mm×4.6 mm,5μm)为分析柱,0.1%(v/v)甲酸水溶液-乙腈为流动相进行梯度洗脱,在电喷雾负离子、目标二级离子扫描模式下进行检测,外标法定量。结果表明,在0.5~100.0 mg/L范围内该分析物的线性关系良好,相关系数为0.999 3,方法的检出限(LOD,S/N≥3)和定量限(LOQ,S/N≥10)分别为3 mg/kg和10 mg/kg。在不同蜂蜜样品中分别添加50.0、100.0、200.0 mg/kg(洋槐蜜中添加10.0、20.0、50.0 mg/kg)特征化合物标准品进行加标回收率试验,平均回收率为82.0%~95.2%,相对标准偏差为2.7%~9.7%(n=6)。利用该方法对来自新西兰12种不同品种的95个蜂巢成熟原蜜和来自4个国家50个商品化蜂蜜进行了验证。该法快速、灵敏、准确,可为解决进口新西兰麦卢卡蜂蜜的判别难题提供技术支持。A method for the determination of characteristic compound3,5-dimethoxybenzoate-4-diglucoside(leptosperin)in manuka honey was developed by automatic on-line solid phase extraction-liquid chromatography-high resolution mass spectrometry(SPE-LC-HRMS).The samples were separated on a Dikma Diamonsil Plus C18column(150mmx4.6mm,5(xm)using the mobile phases of0.1%(v/v)formic acid aqueous solution and acetonitrile with gradient elution.The compound was detected with negative electrospray ionization(ESI-)in Target-MS2mode.The results showed that the linear range was0.5-100.0mg/L,the correla-tion coefficient was0.9993.The limit of detection(LOD,S/N≥3)and limit of quantification(LOQ,S/N≥10)of the method was3mg/kg and10mg/kg,respectively.The recoveries at the spiked levels of50.0,100.0,200.0mg/kg(10.0,20.0,50.0mg/kg in black locust sam-ples)were in the range of82.0%-95.2%with the relative standard deviations ranging from2.7%to9.7%(n=6).The proposed method was applied to95mature honey samples from hives in New Zealand including12different kinds and50commercial honey samples from four different countries.The method is fast,sensitive and accurate to provide technical support to solve the judgment of the manuka honey imported from New Zealand.

关 键 词：全自动在线固相萃取-液相色谱-高分辨质谱 特征标志物 3 5-二甲氧基苯甲酸甲酯-4-双葡萄糖糖苷 麦卢卡蜂蜜 

分 类 号：O658[理学—分析化学]