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Chemistry and Industry of Forest Products ›› 2017, Vol. 37 ›› Issue (5): 93-100.doi: 10.3969/j.issn.0253-2417.2017.05.012

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Gas Chromatographic Methodology and Its Application to Analyze Intermediate Oxalates of Synthetic Borneol

YUAN Xiaomin1, ZHANG Pinghui1, TU Yongyuan2, WANG Jing1,3, LI Dongmei1, ZHAO Zhendong1,3   

  1. 1. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab. for Biomass Chemical Utilization;Key and Open Lab. of Forest Chemical Engineering, SFA;Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;
    2. Fujian Quality Inspection Center for Incense Products, Quanzhou 362600, China;
    3. Research Institute of Forestry New Technology, CAF, Beijing 100091, China
  • Received:2017-03-24 Online:2017-10-25 Published:2017-10-30

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Abstract: While the synthesized difenchyl oxalate(DFO), dibornyl oxalate(DBO), diisobornyl oxalate(DIBO), bornyl isobornyl oxalate(BIBO), bornyl fenchyl oxalate(BFO), and isobornyl fenchyl oxalate(IBFO) were used as reference substances, the qualitative and quantitative analytic methodologies were studied and established for the main intermediates of borneol by gas chromatography(GC), and then an external reference calibration curve method was also established to determine quantitatively difenchyl, dibornyl oxalates or the similar oxalate intermediates. As the results, it was shown that, difenchyl and dibornyl oxalates as reference substances must be dissolved in an inert solvent such as hexane, and the separation performance of the intermediate oxalates may be influenced obviously by the programmed temperature conditions. By means of reference substance addition and chromatogram comparison methods, the intermediate oxalates of synthetic borneol were separated and identified or predicted to be as difenchyl oxalate(DFO), bornyl fenchyl oxalate(BFO), isobornyl fenchyl oxalate(IBFO), dibornyl oxalate(DBO), bornyl isobornyl oxalate(BIBO), diisobornyl oxalate(DIBO) with the retention time of 46.46,49.92,50.75,53.68,54.42 and 54.89 min etc. The calibration curves for fenchyl and dibornyl oxalates were plotted linearly in the ranges of 1-25 g/L and 5-25 g/L as y=93 622x-48 633(r1=0.998 9) and y=99 480x-55 787(r2=0.999 2), by which their mean recoveries were determined as 103.2% and 106.9% with the relative standard deviations(RSDs) 1.72% and 0.76%, respectively. It is considered that the established qualitative GC method and quantitative mathematic equations would supply the demand to determine either qualitative components or quantitative contents of intermediate oxalates in research fields or industry production process. The common peak area normalization method would also be selected for the content determination for convenience.

Key words: synthetic borneol, intermediate oxalates, gas chromatographic methodology, external calibration curve method

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