Abstract
An efficient analytical method was devised for the accurate L-muscone assay in aqueous samples. It involves solid-phase extraction of L-muscone in adsorption mode using XAD-4 as the sorbent and dichloromethane modified with 10% (v/v) methanol as the eluting solvent. The gas chromatographic analysis of the eluate residue dissolved in toluene on a DB-5MS capillary column provided complete resolution of L-muscone from the [[co]]-extracted interferences. The overall method showed excellent linearity ([[r]]2 ≥ 0.9994) in the range of 0.1 to 2.0 μg/mL with good intra- and inter-day precisions (% RSD = 2.5~7.3) and with high extraction recovery rates (≥ 98.1%). When the present method was applied to a L-muscone herbal drink product, the within-batch RE (%) in the labeled concentration (1.5 μg/mL) for the three randomly chosen bottles were -2.4, -1.3 and -3.3 with high precision (% RSD ≤ 3.1). The present method is considered to be suitable for quality control evaluation on liquid drinks and other complex formulations fortified with L-muscone.
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Enoch, P., Putzler, A., Rinne, D., and Schlüter, J., Automated solid-phase extraction on-line coupled to gas chromatography.J. Chromatogr. A, 822, 75–82 (1998).
Filho, I. D. N., Schossler, P., Freitas, L. S., Melecchi, M. I. S., Vale, M. G. R., and Caramão, E. B., Selective extraction of benzoic acid from landfill leachate by solid-phase extraction and ion-exchange chromatography.J. Chromatogr. A, 1027, 167–170 (2004).
Hong, X. and Wang, Z., A preliminary research on the quality of musk.Zhongguo Zhong Yao Za Zhi., Apr; 16 (4), 230–232 (1991).
Jacob, S., Garcia, S. Hayreh, D., and McClintock, M. K., Psychological effects of musky compounds: comparison of androstadienone with androstenol and muscone.Horm. Behav., 42, 274–283 (2002).
Jung, M. W., Ahn, K. H., Lee, Y., Kim, K. P., Paeng, I. R., Rhee, J. S., Park, J. T., and Paeng, K. J., Evaluation on the adsorption capabilities of new chemically modified polymeric adsorbents with protoporphyrin IX.J. Chromatogr. A, 917, 87–93 (2001).
Kamat, V. P., Hagiwara, H., Katsumi, T., Hoshi, T., Suzuki, T., and Ando, M., Ring closing metathesis directed synthesis of (R)-(-)-muscone from (+)-citronellal.Tetrahedron, 56, 4397–4403 (2000).
Kim, K. R., Shin, Y. J., Shim, W. H., and Myung, S. W., Rapid gas chromatographic profiling and screening of acidic nonsteroidal anti-inflammatory drugs in biological samples.Arch. Pharm. Res., 17 (3), 175–181 (1994).
Kim, K. R., Paik, M. J., Kim, J. H., Dong, S. W., and Jeong, D. H., Rapid gas chromatographic profiling and screening of biologically active amines.J. Pharm. Biomed. Anal., 15, 1309–1318 (1997).
Kim, K. R., Park, H. G., Paik, M. J., Ryu, H. S., Oh, K. S., Myung, S. W., and Liebich, H. M., Gas chromatographic profiling and pattern recognition analysis of urinary organic acids from uterine myoma patients and cervical cancer patients.J. Chromatogr. B, 712, 11–22 (1998).
Lee, S. M., Cho, T. S., Shim, S. H., Park, S. K., Hong, C. Y., Kim, S. S., Shin, D. H., Kim, Y. K., and Park, D. K., General pharmacology of L-Muscone.J. Appl. Pharmacol., 5, 292–298 (1997).
Lepane, V., Comparison of XAD-4 resins for the isolation of humic substances from seawater.J. Chromatogr. A, 845, 329–335 (1999).
Vera-Avila, L E., Gallegos-Perez, J. L., and Camacho-Frias, E., Frontal analysis of aqueous of phenol solutions in amberlite XAD-4 columns, Implication on the operation and design of solid-phase extraction system.Talanta, 50, 509–526 (1999).
Vilar, R. B. C., Silva, V. R. da., Schossler, P., Veses, R. C., Piatnicki, C. M. S., Samios, D., and Caramão, E. B., Preliminary characterization of anhydrous ethanol used Brazil as automotive fuel.J. Chromatogr. A, 985, 367–373 (2003).
Wu, Y., Wu, P., Xiao, X., and Yu, D. Q., Method of analysis for musk, artificially bred musk and original musk by HPLC.Yao Xue Xue Bao, 24 (4), 308–311 (1989).
Zhang, Z. H., and Yue, P. F., Quantitative analysis of muscone in musk by GC.Yao Xue Xue Bao, May; 16 (5), 371–378 (1982).
Zou, Q. G. and Su, J. J., Quantitative analysis of muscone in shexiang baoxin pills by gas chromatography.Zhongguo Yao Za Zhi, Jul; 19 (7), 418–419 (1994).
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Paik, MJ., Kim, KR. Solid-phase extraction of l-muscone from aqueous samples with amberlite XAD-4 for gas chromatographic assay. Arch Pharm Res 27, 539–543 (2004). https://doi.org/10.1007/BF02980128
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DOI: https://doi.org/10.1007/BF02980128