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KMID : 0380620070390040372
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Korean Journal of Food Science and Technology
2007 Volume.39 No. 4 p.372 ~ p.379
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Development of Rapid Analytical Method of Forbidden Medicines in Dietary Supplements Using LC-ESI-Tandem MS
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Kim Hee-Yun
Lee Hwa-Mi
Jang Young-Mi
Joo Hyun-Jin
Jung Young-Hyun
Lee Myoung-Sook
Park Jong-Seok
Lee Kwang-Ho
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Abstract
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A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference`s characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.
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KEYWORD
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forbidden medicines, dietary supplements, HPLC/UV, PDE-5 inhibitors, LC-ESI-tandem MS
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