| Clove volatile oil is extracted by steam distillation in the research by orthogonal test. The concrete method is described below : The dry buds of cloves are broken into pieces, then dipped in water at room temperature for 24 hours, and then extracted by ultrasonic wave for 30 minutes. The extract is distilled with steam for 5 hours and the distilled solution is left to delaminate for some minutes. The nether layer of oil is isolated and pure volatile oil of clove is obtained after dehydration by anhydrous Na2SO4.Conditions of GC-MS are described below: the chromatographic column is SGE-30QC3\AC225(0. 32mm × 30m, 0. 25 μ m). The column temperature is programmed from 70℃ to 160℃ at 6℃ ? min-1 and then to190℃ at 3℃ ? min-1. The injected volume is 0. 5 μL. The pressure before column is 60kpa. They explore the accuracy, fidelity and stability of instrument and analyze the fingerprint spectrum of volatile oil extracted from ten batches of cloves.The accuracy, fidelity and stability of instrument are very good in the tests with the RSD of the relative retention time and area of common peaks smaller than 3%. They match the spectrum and peaks , and calculate the similarity by data processing function of Excel 2002 which is one of the office software of Microsoft Office, and establish the common fingerprint spectrum of clove volatile oil and it meets the requirement of fingerprint spectrum that the similarity of ten batches of cloves is more than 0. 99 .They optimize the conditions and acquire the chromatogram conditions with high sensitivity and proper pre-treatment method . The analysis method of clove volatile oil established by GC-MS has good fidelity, accuracy and stability, and at the same time, the method of GC-MS has the advantage in qualitative analysis of various components simultaneously. As a result, the fingerprint spectrum established here can offer a reference for quality control of clove and make a basis for Chinese traditional medicine fingerprint spectrum establishment. |
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