Chinese Journal of Chromatography

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

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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).

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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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