Simultaneous Identification of Hydroxythiohomosildenafil, Aminotadalafil, Thiosildenafil, Dimethylsildenafil, and Thiodimethylsildenafil in Dietary Supplements Using High-Performance Liquid Chromatography-Mass Spectrometry

貴臣, 田上; 章弘, 武田; 安紀子, 淺田; 愛倫, 青山; 崇広, 土井; 計志, 梶村; 善之, 沢辺

doi:10.3358/shokueishi.54.232

Cited by 7 publications

(3 citation statements)

References 8 publications

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“…Kee et al [16] achieved the classification of two sets of isomers (sildenafil analogues and mercaptosidinafil analogues) by Orbitrap mass spectrometry (MS) method, and the database of these compounds was established using quality processing software. Tagami et al [17] established a method for the isolation and identification of five sildenafil analogues using liquid chromatography-mass spectrometry (LC-MS). Huang et al [18] achieved the qualitative and quantitative detection of 17 kidney-tonifying and yang-strengthening chemicals that were illegally added in Chinese patent medicine by LC-MS method.…”

Section: Introductionmentioning

confidence: 99%

Rapid and Quantitative Determination of Sildenafil in Cocktail Based on Surface Enhanced Raman Spectroscopy

Lin

Nie

et al. 2019

Molecules

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Sildenafil (SD) and its related compounds are the most common adulterants found in herbal preparations used as sexual enhancer or man’s virility products. However, the abuse of SD threatens human health such as through headache, back pain, rhinitis, etc. Therefore, it is important to accurately detect the presence of SD in alcoholic beverages. In this study, the Opto Trace Raman 202 (OTR 202) was used as a surface-enhanced Raman spectroscopy (SERS) active colloids to detect SD. The results demonstrated that the limit of detection (LOD) of SD was found to be as low as 0.1 mg/L. Moreover, 1235, 1401, 1530, and 1584 cm−1 could be qualitatively determined as SD characteristic peaks. In a practical application, SD in cocktail could be easily detected using SERS based on OTR 202. Also, there was a good linear correlation between the intensity of Raman peaks at 1235, 1401, 1530, and 1584 cm−1 and the logarithm of SD concentration in cocktail was in the range of 0.1–10 mg/L (0.9822 < R2 < 0.9860). The relative standard deviation (RSD) was less than 12.7% and the recovery ranged from 93.0%–105.8%. Moreover, the original 500–1700 cm−1 SERS spectra were pretreated and the partial least squares (PLS) was applied to establish the prediction model between SERS spectra and SD content in cocktail and the highest determination coefficient (Rp2) reached 0.9856. In summary, the SD in cocktail could be rapidly and quantitatively determined by SERS, which was beneficial to provide a rapid and accurate scheme for the detection of SD in alcoholic beverages.

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Section: Introductionmentioning

confidence: 99%

Rapid and Quantitative Determination of Sildenafil in Cocktail Based on Surface Enhanced Raman Spectroscopy

Lin

Nie

et al. 2019

Molecules

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“…A relatively large number of analysis methods targeting PDE-5 inhibitors have been reported for supplements containing ergogenic ingredients [2][3][4]. However, although many analytical methods targeting individual slimming pharmaceutical ingredients have been reported, there are few methods to analyze many ingredients simultaneously.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Slimming Drugs in Dietary Supplements by Liquid Chromatography/Time-of-Flight Mass Spectrometry

et al. 2019

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A method for the simultaneous determination of 13 slimming drugs in dietary supplements by liquid chromatography/time-of-flight mass spectrometry was developed and applied to real-time surveys of imported health supplements. The target compounds were mutually well separated on a reversed-phase LC Shodex ODP2-HP 2D column using a combination of step-wise and linear gradient elution of a mixed mobile phase solution of ammonium formate buffer, methanol, and formic acid. The detection limits were in the range 1-50 ng/mL, and the lower limits of quantification were 2-100 ng/mL. The average recoveries of the 13 types of pharmaceutical ingredients in the diet supplements were 93-110%, and the RSD was within 7.1%. Applying the developed method to the survey of imported dietary supplements revealed that 32 out of the 39 Chinese products tested contained pharmaceutical ingredients such as sibutramine. On the other hand, out of 30 US products, synephrine was detected in 26 specimens, and yohimbine was detected in 8 specimens. These results proved that a number of products were contaminated by drugs, which was considered to be intentional. The developed method is applicable for the survey of imported health supplements suspected to be contaminated with pharmaceutical ingredients.

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“…The detection processes of TCM ingredients are complicated and challenging. Several methods are used to determine undeclared adulterants in herbal medicine or food supplements, including the following: LC-PDA [ 12 ], GC-MS [ 13 ], GC-QQQMS [ 14 ], LC-MS [ 15 ], LC-MS/MS [ 12 ], UPLC-TOF/MS [ 16 ], Q-Orbitrap MS [ 17 ], NMR [ 18 ], X-ray powder diffractometry [ 19 ], TLC-image [ 20 ], TLC-SERS [ 21 ], ATR‑IR [ 22 ], and CE-MS [ 23 ]. The applicability of GC‑MS is determined by the volatility and thermal stability of analytes.…”

Section: Introductionmentioning

confidence: 99%

Detection of adulterated drugs in traditional Chinese medicine and dietary supplements using hydrogen as a carrier gas

et al. 2018

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Helium, a minor component of natural gas and radioactive minerals, is most commonly used as a carrier in gas chromatography-mass spectrometry (GC-MS). Its scarcity leads to limited availability and higher costs. In this experiment, hydrogen from a safe source of a hydrogen generator was tested as a substitutive carrier gas for the detection of adulterant in traditional Chinese medicine (TCM) and food supplements by GC-MS analysis. We found that the limits of detection (LODs) of using hydrogen were from 10 to 1000 μg/g. The levels of LODs tested among 170 drugs remain the same whether hydrogen or helium was used as a carrier gas with the exception of 7 drugs—benzbromarone, estradiol benzoate, bezafibrate, mefenamic acid, oxymetholone, piperidenafil and cetilistat. The real sample analysis results using hydrogen were as satisfactory as those using helium. In addition, the retention time was shortened after the chromatographic performance was optimized. In summary, it is worth considering hydrogen as a carrier gas due to its affordable costs, energy efficiency, carbon reduction and chromatographic advantages to detect adulterated drugs in TCM and dietary supplement using GC-MS.

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Simultaneous Identification of Hydroxythiohomosildenafil, Aminotadalafil, Thiosildenafil, Dimethylsildenafil, and Thiodimethylsildenafil in Dietary Supplements Using High-Performance Liquid Chromatography-Mass Spectrometry

Cited by 7 publications

References 8 publications

Rapid and Quantitative Determination of Sildenafil in Cocktail Based on Surface Enhanced Raman Spectroscopy

Rapid and Quantitative Determination of Sildenafil in Cocktail Based on Surface Enhanced Raman Spectroscopy

Simultaneous Determination of Slimming Drugs in Dietary Supplements by Liquid Chromatography/Time-of-Flight Mass Spectrometry

Detection of adulterated drugs in traditional Chinese medicine and dietary supplements using hydrogen as a carrier gas

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