A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification
Objective: This study is aimed to develop a qualitative and quantitative method to detect a novel vardenafil analogue from a healthcare product, which is claimed to enhance sexual function. Method: The unknown compound was detected by non-targeted screening using ultra-high performance liquid chroma...
| Main Authors: | , , , |
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| Format: | Article |
| Language: | English |
| Published: |
Elsevier
2023-09-01
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| Series: | Heliyon |
| Subjects: | |
| Online Access: | http://www.sciencedirect.com/science/article/pii/S2405844023066641 |
| _version_ | 1797669843225280512 |
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| author | Jintao Xia Wanqin Wu Feng Jiang Songsong Zhu |
| author_facet | Jintao Xia Wanqin Wu Feng Jiang Songsong Zhu |
| author_sort | Jintao Xia |
| collection | DOAJ |
| description | Objective: This study is aimed to develop a qualitative and quantitative method to detect a novel vardenafil analogue from a healthcare product, which is claimed to enhance sexual function. Method: The unknown compound was detected by non-targeted screening using ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS). MS2 spectra showed that the characteristic fragment ions of this unknown compound were highly similar to those of vardenafil. This compound was subsequently isolated by silica gel column chromatography and characterized by 1D (dimension) and 2D nuclear magnet resonance (NMR) specta, ultra-violet (UV) spectra, and fourier transform infrared (IR) spectra. A quantitative method for analyzing this identified compound in various healthcare product was developed based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Results: The unknown compound was identified as 2-(5-((4-ethylpiperazin-1-yl)sulfonyl)-2-propoxyphenyl)-5-methyl-7-propylimidazo.[5,1-f] [1,2,4]triazin-4(3H)-one based on the spectroscopic data. Quantitative results revealed that the matrix calibration curves of this compound had a good linear ranges of 2～50 ng/mL in pressed candy (R2 = 0.998), energy coffee (R2 = 0.999), and health wine (R2 = 0.997), respectively. The matrix effects, recoveries, and limit of quantitation (LOQ) of this compound all met the requirements of quantitative validation. Finally, the content of this compound in 5 batches of positive samples ranged from 1.24 to 7.20 g/kg. Conclusion: This study identified a novel vardenafil analog from a healthcare product and named it O-propyl vardenafil, and this compound was distinguished from vardenafil by the replacement of the ethyl group with a propyl group at the aryl alkyl ether moiety. Our developed quantitative method could meet practical needs. The high positive rate (16.67%) in 30 samples suggested that the related regulators should be alert to O-propyl vardenafil in routine test since it has not been detected ever before. |
| first_indexed | 2024-03-11T20:50:40Z |
| format | Article |
| id | doaj.art-78447058b7684fd3896a0f894ca8b343 |
| institution | Directory Open Access Journal |
| issn | 2405-8440 |
| language | English |
| last_indexed | 2024-03-11T20:50:40Z |
| publishDate | 2023-09-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Heliyon |
| spelling | doaj.art-78447058b7684fd3896a0f894ca8b3432023-10-01T05:59:43ZengElsevierHeliyon2405-84402023-09-0199e19456A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantificationJintao Xia0Wanqin Wu1Feng Jiang2Songsong Zhu3Hubei Provincial Institute for Food Supervision and Test, Wuhan 430075, China; Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Wuhan 430075, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, China; Corresponding author. Hubei Provincial Institute for Food Supervision and Test, No. 8 Yaojian 2th Road, Wuhan East Lake High-tech Development Zone, Wuhan 430075, China.Hubei Provincial Institute for Food Supervision and Test, Wuhan 430075, China; Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Wuhan 430075, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, ChinaHubei Provincial Institute for Food Supervision and Test, Wuhan 430075, China; Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Wuhan 430075, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, ChinaHubei Provincial Institute for Food Supervision and Test, Wuhan 430075, China; Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Wuhan 430075, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, ChinaObjective: This study is aimed to develop a qualitative and quantitative method to detect a novel vardenafil analogue from a healthcare product, which is claimed to enhance sexual function. Method: The unknown compound was detected by non-targeted screening using ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS). MS2 spectra showed that the characteristic fragment ions of this unknown compound were highly similar to those of vardenafil. This compound was subsequently isolated by silica gel column chromatography and characterized by 1D (dimension) and 2D nuclear magnet resonance (NMR) specta, ultra-violet (UV) spectra, and fourier transform infrared (IR) spectra. A quantitative method for analyzing this identified compound in various healthcare product was developed based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Results: The unknown compound was identified as 2-(5-((4-ethylpiperazin-1-yl)sulfonyl)-2-propoxyphenyl)-5-methyl-7-propylimidazo.[5,1-f] [1,2,4]triazin-4(3H)-one based on the spectroscopic data. Quantitative results revealed that the matrix calibration curves of this compound had a good linear ranges of 2～50 ng/mL in pressed candy (R2 = 0.998), energy coffee (R2 = 0.999), and health wine (R2 = 0.997), respectively. The matrix effects, recoveries, and limit of quantitation (LOQ) of this compound all met the requirements of quantitative validation. Finally, the content of this compound in 5 batches of positive samples ranged from 1.24 to 7.20 g/kg. Conclusion: This study identified a novel vardenafil analog from a healthcare product and named it O-propyl vardenafil, and this compound was distinguished from vardenafil by the replacement of the ethyl group with a propyl group at the aryl alkyl ether moiety. Our developed quantitative method could meet practical needs. The high positive rate (16.67%) in 30 samples suggested that the related regulators should be alert to O-propyl vardenafil in routine test since it has not been detected ever before.http://www.sciencedirect.com/science/article/pii/S2405844023066641Healthcare productHRMSNMRQuantitative analysisVardenafil analog |
| spellingShingle | Jintao Xia Wanqin Wu Feng Jiang Songsong Zhu A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification Heliyon Healthcare product HRMS NMR Quantitative analysis Vardenafil analog |
| title | A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification |
| title_full | A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification |
| title_fullStr | A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification |
| title_full_unstemmed | A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification |
| title_short | A novel vardenafil analog in a healthcare product: Preparation, characterization, and quantification |
| title_sort | novel vardenafil analog in a healthcare product preparation characterization and quantification |
| topic | Healthcare product HRMS NMR Quantitative analysis Vardenafil analog |
| url | http://www.sciencedirect.com/science/article/pii/S2405844023066641 |
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