• Mass Spectrometry Letters
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• v.3 no.2
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• pp.50-53
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• 2012

After success of sildenafil for the treatment of erectile dysfunction, a large number of its analogues have been approved from FDA. Recently, the illegal dietary supplements which include sildenafil, vardenafil, tadalafil, or analogues of these drugs as ingredient have been widely distributed. Therefore, the determination of the residue of synthetic phosphodiesterase- 5 (PDE-5) inhibitors in dietary supplements is highly required due to indiscriminate and unintentional overdose caused nausea, chest pains, fainting and irregular heartbeat. In this paper, we report a rapid and sensitive analytical method for the simultaneous determination of nine phosphodiesterase-5 inhibitors by liquid chromatography-high resolution mass spectrometry. The present method was found to be accurate and reproducible with 40 ${\mu}g$/g of the limit of quantification for the nine PDE-5 inhibitors. The developed method can be successfully applied to the analysis of the seven illegal dietary supplements.

• Korean Journal of Biological Psychiatry
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• v.13 no.4
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• pp.252-259
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• 2006

Sexual dysfunction is a relatively common adverse effect in the use of antidepressants. The sexual side effects may result in a lack of compliance with the prescribed antidepressants. The author reviewed the prevalence and updated treatment for the antidepressant-induced adverse effects focusing on sexual dysfunction. The incidence of sexual dysfunction is reported to exceed more than 50% especially with SSRIs. In order to obtain a quantified baseline and as an ongoing evaluation tool, clinicians may use some of the established questionnaires and validated instruments such as the Arizona Sexual Experience scale and Changes in Sexual Functioning Questionnaire. Clinicians should be aware that delayed ejaculation and orgasm, symptoms most frequently associated with antidepressants, are not usually associated with depression itself. Although many antidotes have been proposed, few have been subjected to double-blind trials. Some evidences have suggested that bupropion and buspiron may be the effective antidotes for SSRI induced sexual dysfunction. Additional trials will be requied to define what role, if any, bupropion and buspiron might have in the treatment of SSRI-induced sexual side effects. The available evidence is rather limited, with only small number of trials assessing each strategy. While further randomized data is awaited, for men with antidepressant induced erectile dysfunction, the addition of sidenafil or tadalafil may appear to be an effective strategy.

• Journal of environmental and Sanitary engineering
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• v.22 no.3
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• pp.89-96
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• 2007

To determine 8 anti-impotence drug/drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil, aminotadalafil, pseudovardenafil and hongdenafil in foods, simultaneously, high performance liquid chromatography(HPLC) and liquid chromatography-mass spectrometry (LC/MS) were used. The HPLC/UV analysis was performed on a column of capcellpak $C_{18}$ with 0.1% sodium-1-hexansulfonate in 0.2M ammonium formate/acetonitrile as a mobile phase. Mass spectra of the compounds by LC/MS were investigated with SCAN mode(Mass range and Fragment voltage) and SIM(Selected Ion Monitoring) mode (Ion target and Fragment voltage). The results follow as; 1. The HPLC/UV analysis was detected from 5 out of 63 samples. The content of sildenafil was in the range of 32.80 ppm ${\sim}$ 60.13 ppm from 4 out of 5 samples. The contents of sildenafil, vardenafil, homosildenafil were in the range 47.14 ppm from 1 out of 5 samples. 2. The conformed result of LC/MS was equal of detected from 5 out of 63 samples in HPLC/UV analysis. An easily available, simultaneous determination of 8 standards in adulterated health related foods was established by using a combination of LC/MS methods.

• Mass Spectrometry Letters
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• v.13 no.3
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• pp.58-83
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• 2022

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL^-1; linearity (r²) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL^-1, linearity (r²) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

• Analytical Science and Technology
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• v.20 no.1
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• pp.78-83
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• 2007

To perform proficiency test for determining anti-impotence drug-like compounds in food, interlaboratory test has been done. Targets were 6 such as sildenafil, tadalafil, vardenafil, homosildenafil, hydroxy-homosildenafil and pseudo-vardenafilI. Total 13 institutes were participated and all is in charging of food analysis. To do double blind test, the reference materials were made as 13 different ginseng drink samples and each sample had random 3 targets. By the official method for anti-impotence drug-like compounds in food code, sample was just diluted in water, extracted in organic solvents, determined by HPLC/UV and then confirmed by LC/MS. The analytical duration was 60 days after receiving sample. Ten out of 13 institutes were satisfied by evaluation of Z-score and RSZ according to the regulation for managing analytical quality assurance.

• Korean Journal of Food Science and Technology
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• v.48 no.5
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• pp.405-412
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• 2016

Illegally adulterated compounds, such as impotency drugs and their synthetic analogues, which have been purported to enhance sexual potency or mood, have been constantly detected in foods including dietary supplements. The adulterated foods with these illegal compounds may threaten public health because their safety and efficacy have not been verified. This study was aimed at investigating illegal compounds in foods and counterfeit products. 54 illegal compounds were assayed using a simultaneous analytical method involving liquid chromatography equipped with photo diode array (LC-PDA) and LC coupled with tandem mass spectrometry (LC-MS/MS). The method was validated in terms of selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision and accuracy. In 48 of 161 samples, we identified 7 different illegal compounds, including sildenafil, tadalafil, chlropretadalafil, demethylsildenafil, dimethyl-thiosildenafil, icariin and yohimbine. When purchasing products marketed for erectile dysfunction or aphrodisiacs, ulmost care should be taken owing to the possible presence of these illegal compounds.