Determination of Curcumol in Baofu Kangshuan by Capillary Gas Chromatography - Master's thesis - Dissertation

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This study presents a method for determining the curcumol content in Baofukang suppository using capillary gas chromatography. Baofukang is a traditional Chinese medicine formulation included in the Chinese Pharmacopoeia, containing zedoary turmeric oil and borneol. Among the active compounds in zedoary turmeric oil, such as elemene, curcumol, and zedoary diketone, are known for their anti-inflammatory, antibacterial, and anticancer properties. However, these components have not been quantitatively analyzed in the current pharmacopoeia standards. This paper introduces a reliable and accurate capillary gas chromatographic method to quantify curcumol, thereby enhancing the quality control of the preparation.

The method involves the use of a Puri GC7800 gas chromatograph equipped with a SE30 capillary column (30m × 0.25mm × 0.25μm). The analysis was performed under programmed temperature conditions, starting at 130°C for 40 minutes, then increasing at 32°C/min to 250°C for 16 minutes. A flame ionization detector (FID) was used with a carrier gas of nitrogen at a pressure of 0.5 kg/cm². The injection port and detector temperatures were both set to 280°C. The split ratio was 1:100. The theoretical plate count was verified to be no less than 25,000 based on the zedoary alcohol peak.

For the internal standard solution, n-tridecane and ethyl acetate were prepared at a concentration of 1 mg/mL. Calibration factors were determined by preparing a solution of 3 mg curcumol in 10 mL volumetric flask, adding 2 mL of the internal standard, and diluting to volume with ethyl acetate. A 1 μL aliquot was injected into the gas chromatograph, and the average peak area was calculated over 3–5 injections.

The test solution was prepared by extracting volatile oils from 10 samples of the suppository using ethyl acetate. After three extractions, the combined ethyl acetate layer was diluted and mixed with the internal standard solution. The resulting solution was analyzed by gas chromatography. The method showed good specificity, with no interference from other components in the blank sample. The separation between curcumol and the internal standard was greater than 1.5, and all peaks were symmetric.

A linear relationship was established by preparing a series of standard solutions with concentrations ranging from 0.1 to 0.5 mg/mL. The regression equation obtained was Y = 3.54X - 2.48×10⁻³, with a correlation coefficient r = 0.9995. Recovery tests showed an average recovery rate of 102.3%, with RSD = 2.92%. The method also demonstrated good precision, with an RSD of 2.6% across five repeated injections. Repeatability testing yielded an RSD of 2.9%. Three batches of samples were analyzed following the same procedure.

In conclusion, this method provides a simple, accurate, and reproducible way to determine curcumol content in Baofukang suppository, contributing to improved quality control of the product. Further studies may explore the simultaneous analysis of other compounds like borneol, especially if multi-stage temperature-programmed chromatography is available. The results demonstrate the potential of gas chromatography for the quantitative analysis of herbal preparations.

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