• Analytical Science and Technology
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• v.16 no.6
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• pp.488-498
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• 2003

By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.

• The Korea Journal of Herbology
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• v.30 no.6
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• pp.69-75
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• 2015

Objectives : This study was designed to investigate effects of the combination with Korean Red Ginseng (Panax ginseng C.A. Meyer), Gastrodia Rhizoma (Gastrodia elata Blume) and Polygoni Multiflori Radix (Polygonum multiflorum Thunberg) on metabolic disorders including cholesterol and erectile dysfunction in hyperlipidemia rats.Methods : Animals were divided into six groups; Control with normal diet, high fat/cholesterol-diet (HFCD), fluvastatin, Korean Red Ginseng treated (KRG), and the combination treated (Korean Red Ginseng, Gastrodia Rhizoma and Polygoni Multiflori Radix; 1:1:1 for KGP1 and 2:1:1 for KGP2). The experimental groups initially received HFCD for 10 weeks and then treated orally with fluvastatin, KRG, KGP1 and KGP2 during the final 6 weeks. Erectile function was determined by the measurements of intracavernosal pressure (ICP) and maximal arterial pressure (MAP) after electrical stimulation of the cavernosal nerve.Results : KGP2 decreased the level of total cholesterol and LDL cholesterol in the sera of HFCD rats without no changes of body weights. KRG, KGP1 and KGP2 decreased the level of C-reactive protein (CRP) levels except of fluvastatin, synthetic HMG-CoA reductase inhibitor. KRG, KGP1 and KGP2 significantly increased the ICP, ICP/MAP ratio, area under the curve (AUC) compared with those of normal rat. Morphometric analyses showed that KRG, KGP1 and KGP2 increased the volume of smooth muscle and the regular arrangement of collagen fibers in corpus cavernosum of HFCD rats. The penile expression of eNOS was increased by KRG, KGP1 and KGP2.Conclusions : Based on these results, we suggest that the combination with Korean Red Ginseng, Gastrodia Rhizoma and Polygoni Multiflori may improve hyperlipidemia through regulating the lipid profiles and erectile dysfunction in rats.

• Analytical Science and Technology
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• v.28 no.4
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• pp.278-287
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• 2015

Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction. In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatography-quadrupole-time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions. Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.

• Analytical Science and Technology
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• v.22 no.2
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• pp.172-185
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• 2009

To help understanding about hazard chemicals occurring newly in food, it has been reviewed characteristics, mechanism, food standards and analytical trend of the hazard chemicals occurring avoidably in food manufacturing process. The new hazard chemicals in food are classified by 4 regarding mechanism such as heat, fermentation, additives and unknowns. The new hazard chemicals by heat process are acrylamide, furan, HCAs and PAHs. By the fermentation, ethylcarbamate and biogenic amines are occurred. According to food additives, 3-MCPD, benzene and nitrosamines can be produced. And the last group is the illegal compounds including anti-impotence drug analogues and anti-obesity drug analogues. To analyze the new hazard chemicals in food, GC or LC with UVD, FLD or MSD are used mainly after sample pretreatment by LLE, SPE or headspace method.

• Journal of Food Hygiene and Safety
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• v.30 no.1
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• pp.35-42
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• 2015

This study was performed for both evaluating the safety of other processed products and providing basic information for making the general standard for contaminants in the category of other processed products. We analyzed the contents of three heavy metals, thirty six anti-impotence drugs and their analogues, three anti-obesity drugs and their analogues, twenty eight steroid drugs and their analogues, collecting in Incheon Metropolitan City. Any illegal compound was not detected in those products. However the contents of lead, cadmium and mercury of those products were at the range of 0.001-13.390 mg/kg, 0.03-1.231 mg/kg and 0.001-0.650 mg/kg respectively. Because there are no standards of heavy metals against other processed products, we compared the analytical results with relevant standards of both S. Korea and foreign countries. As a result, two products exceeded the relevant standards of lead, and other two products exceeded the relevant standards of mercury. The relative hazards compared to PTWI of FAO/WHO (Codex), Seafoods-pajeonmix, Perilla seed powder exceeded PTWI standards 0.214. The compulsory standards of each food product are determined by the category of the products. Because there is no standard of heavy metals in the category of other processed products in S. Korea, any food products registered as other processed product by manufacturer are free with those standards. Abusing similar problems on the categorization of food products could cause consumers' health problem. To prevent these problems, detail regulations on the categorization of food products have to be introduced.

• Korean Journal of Food Science and Technology
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• v.44 no.2
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• pp.148-154
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• 2012

It was carried out to detect anti-impotence drug-like compounds, sibutramine and their analogues in dietary supplements, which are doubtful whether they include illegal compounds. A total of 51 food products were bought online and have been investigated. The separation was achieved on a C18 column, with the mobile phase made up of water (5 mM sodium hexanesulfonate and 0.1% phosphoric acid) and 95% acetonitrile, at a flow rate of 1.2 mL/min with gradient elution using by HPLC-DAD. The UV signals were monitored at 220 nm and 291 nm. LC-ESI-tandom MS was utilized to confirm that detected compounds in samples are the same as the reference materials. Two nutrient supplement foods and ginseng products were found to contain 1.3-82.1 mg of sildenafil, dimethylthiolsildenafil and pseudovardenafil per serving size. In addition, two other processed products were detected to contain 1.7 and 2.2 mg of didesmethylsibutramine, derived from sibutramine per serving size.