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Molecules 2013, 18(2), 1368-1382; doi:10.3390/molecules18021368

Article

Profiling and Characterization of Volatile Components from Non-Fumigated and Sulfur-Fumigated Flos Lonicerae Japonicae Using Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry Coupled with Chemical Group Separation

Hao Cai ^1,2,3,†,* , Gang Cao ^2,3,4,† , Li Li ^5,† , Xiao Liu ^1,2,3 , Xiao-Qing Ma ^1,2 , Si-Cong Tu ⁶ , Ya-Jing Lou ^1,2 , Kun-Ming Qin ^1,2 , Song-Lin Li ⁷  and Bao-Chang Cai ^1,2,3,4,*

¹ Department of Chinese Materia Medica, College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China ² Engineering Center of State Ministry of Education for Standardization of Chinese Medicine Processing, Nanjing University of Chinese Medicine, Nanjing 210023, China ³ National First-Class Key Discipline for Science of Chinese Materia Medica, Nanjing University of Chinese Medicine, Nanjing 210023, China ⁴ Research Center of TCM Processing Technology, Zhejiang Chinese Medical University, Hangzhou 310053, China ⁵ LECO Corporation Shanghai Representative Office, Shanghai 201900, China ⁶ Faculty of Medicine, University of New South Wales, Sydney, NSW 2031, Australia ⁷ Department of Pharmaceutical Analysis and Metabolomics, Jiangsu Province Academy of Chinese Medicine, Nanjing 210028, China ^† These authors contributed equally to this work.

* Authors to whom correspondence should be addressed.

Received: 25 October 2012; in revised form: 10 January 2013 / Accepted: 14 January 2013 / Published: 24 January 2013

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Abstract: Flos Lonicerae Japonicae (FLJ) is a popular herb used for many centuries in Traditional Chinese Medicine as a treatment of fever and inflammation. Non-fumigated processing of FLJ has been the traditional approach used in post-harvest preparation of the commodity for commercial use. However, in recent years, natural drying processing of FLJ has been replaced by sulfur-fumigation for efficiency and pest control. Sulfur-fumigation can induce changes in the volatile compounds of the herb, altering its medicinal properties. A comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF/MS) method was established for the resolution and determination of volatile components in non-fumigated and sulfur-fumigated FLJ. In this paper, analysis of the volatile oils in non-fumigated and sulfur-fumigated (including lab-prepared sulfur- fumigated and industrial sulfur-fumigated) FLJ was performed using GC×GC-TOF/MS. Seventy-three representative volatile components were identified, including furans, alkalies, acids, aldehydes, ketones, alcohols, terpenes, esters, and others, as the main components of FLJ volatile oils. The proposed method was successfully applied for rapid and accurate quality evaluation of FLJ and its related medicinal materials and preparations.

Keywords: sulfur-fumigation; GC×GC-TOF/MS; volatile compounds; Flos Lonicerae Japonicae; quality control

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