色谱 ›› 2017, Vol. 35 ›› Issue (10): 1068-1072.DOI: 10.3724/SP.J.1123.2017.07009

• 研究论文 • 上一篇    下一篇

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

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5   

  1. 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
  • 收稿日期:2017-07-10 出版日期:2017-10-08 发布日期:2017-10-18
  • 通讯作者: 丁涛,E-mail:dingt@jsciq.gov.cn.
  • 基金资助:

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

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

SHEN Chongyu1, GUO Siyan2, DING Tao1, LIU Yun1, CHEN Lei1, FEI Xiaoqing1, ZHANG Rui1, WU Bin1, SHEN Weijian1, CHEN Lei1, ZHANG Feng3, FENG Feng3, DENG Xiaojun4, YI Xionghai4, YANG Gongjun2, CHEN Guoqiang5   

  1. 1. Animal, Plant and Food Inspection Center, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    2. College of Pharmacy, China Pharmaceutical University, Nanjing 211198, China;
    3. Chinese Academy of Inspection and Quarantine, Beijing 102600, China;
    4. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    5. Suzhou Entry-Exit Inspection and Quarantine Bureau, Suzhou 215004, China
  • Received:2017-07-10 Online:2017-10-08 Published:2017-10-18
  • Supported by:

    National Key Research and Development Plan (No. 2017YFF0211000); Shanghai Yangtze River Delta Science and Technology Cooperation Project (No. 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 C18色谱柱(150 mm×4.6 mm, 5 μm)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0.9993,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。

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

Abstract:

A method for the determination of characteristic compound 3,5-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 C18 column (150 mm×4.6 mm, 5 μm) using the mobile phases of 0.1% (v/v) formic acid aqueous solution and acetonitrile with gradient elution. The compound was detected with negative electrospray ionization (ESI-) in Target-MS2 mode. The results showed that the linear range was 0.5-100.0 mg/L, the correlation coefficient was 0.9993. The limit of detection (LOD, S/N ≥ 3) and limit of quantification (LOQ, S/N ≥ 10) of the method was 3 mg/kg and 10 mg/kg, respectively. The recoveries at the spiked levels of 50.0, 100.0, 200.0 mg/kg (10.0, 20.0, 50.0 mg/kg in black locust samples) were in the range of 82.0%-95.2% with the relative standard deviations ranging from 2.7% to 9.7% (n=6). The proposed method was applied to 95 mature honey samples from hives in New Zealand including 12 different kinds and 50 commercial 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.

Key words: 3,5-dimethoxybenzoate-4-diglucoside (leptosperin), automatic on-line solid phase extraction-liquid chromatography-high resolution mass spectrometry (SPE-LC-HRMS), characteristic compound, manuka honey

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