The Experts below are selected from a list of 315 Experts worldwide ranked by ideXlab platform
Sun Young Baek - One of the best experts on this subject based on the ideXlab platform.
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development and validation of rapid and simultaneous method for determination of 12 hair growth compounds in Adulterated Products by uhplc ms ms
Forensic Science International, 2018Co-Authors: Han Na Park, Sun Young Baek, Sungkwan Park, Hoil KangAbstract:Abstract Synthetic hair-growth compounds have been illegally used in diverse Products to enhance the short-term efficacy of these Products. In this study, a rapid and simultaneous method for the determination of hair-growth compounds in Adulterated Products based on ultra high pressure liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) was developed and validated. The limit of detection (LOD) and limit of quantitation (LOQs) of the method were 0.08–43.6 ng/mL and 0.27–145 ng/mL for the solid-, liquid-, and cream-type samples, respectively. Good calibration linearity for all compounds was demonstrated with a correlation coefficient (r2) higher than 0.997. The intra- and inter-assay precisions were within 11%. The corresponding accuracies were 86–117% and 81–113%, respectively. The mean recoveries obtained for the solid-, liquid, and cream-type samples ranged from 87 to 114%, with a relative standard deviation (RSD) within 6%. The RSD of the stability evaluated at 4 °C for 48 h was less than 6%. The established method was used to screen 76 samples advertised as hair-growth treatments, from online and offline markets, over the course of two years. In 10% of the samples, four compounds, including triaminodil, minoxidil, finasteride, methyltestosterone, and testosterone–propionate were detected. The concentrations were in the range of 0.5–16.4 mg/g. This technique provides a reliable platform for technical analysis for continuous monitoring of Adulterated Products to protect public health.
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simultaneous analysis by quadrupole orbitrap mass spectrometry and uhplc ms ms for the determination of sedative hypnotics and sleep inducers in Adulterated Products
IEEE Journal of Solid-state Circuits, 2017Co-Authors: Han Na Park, Ji Yeon Choi, Hyungjoon Park, Seong Soo Park, Sun Young BaekAbstract:Adulterated Products are continuously detected in society and cause problems. In this study, we developed and validated a method for determining synthetic sedative-hypnotics and sleep inducers, including barbital, benzodiazepam, zolpidem, and first-generation antihistamines, in Adulterated Products using Quadrupole-Orbitrap mass spectrometry and ultrahigh performance liquid chromatography with tandem mass spectrometry. In Quadrupole-Orbitrap mass spectrometry analysis, target compounds were confirmed using a combination of retention time, mass tolerance, mass accuracy, and fragment ions. For quantification, several validation parameters were employed using ultrahigh performance liquid chromatography with tandem mass spectrometry. The limit of detection and limit of quantitation was 0.05-53 and 0.17-177 ng/mL, respectively. The correlation coefficient for linearity was more than 0.995. The intra- and interassay accuracies were 86-110 and 84-111%, respectively. Their precision values were evaluated as within 4.0 (intraday) and 10.7% (interday). Mean recoveries of target compounds in Adulterated Products ranged from 85 to 116%. The relative standard deviation of stability was less than 10.7% at 4°C for 48 h. The 144 Adulterated Products obtained over 3 years (2014-2016) from online and in-person vendors were tested using established methods. After rapidly screening with Quadrupole-Orbitrap mass spectrometry, the detected samples were quantified using ultrahigh performance liquid chromatography with tandem mass spectrometry. Two of them were Adulterated with phenobarbital.
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Simultaneous analysis by Quadrupole‐Orbitrap mass spectrometry and UHPLC‐MS/MS for the determination of sedative‐hypnotics and sleep inducers in Adulterated Products
Journal of Separation Science, 2017Co-Authors: Han Na Park, Ji Yeon Choi, Hyungjoon Park, Seong Soo Park, Sun Young BaekAbstract:Adulterated Products are continuously detected in society and cause problems. In this study, we developed and validated a method for determining synthetic sedative-hypnotics and sleep inducers, including barbital, benzodiazepam, zolpidem, and first-generation antihistamines, in Adulterated Products using Quadrupole-Orbitrap mass spectrometry and ultra high performance liquid chromatography with tandem mass spectrometry. In Quadrupole-Orbitrap mass spectrometry analysis, target compounds were confirmed using a combination of retention time, mass tolerance, mass accuracy, and fragment ions. For quantification, several validation parameters were employed using ultra high performance liquid chromatography with tandem mass spectrometry. The limit of detection and limit of quantitation was 0.05–53 and 0.17–177 ng/mL, respectively. The correlation coefficient for linearity was more than 0.995. The intra- and inter-assay accuracies were 86–110 and 84–111%, respectively. Their precision values were evaluated as within 4.0 (intra-day) and 10.7% (inter-day). Mean recoveries of target compounds in Adulterated Products ranged from 85 to 116%. The relative SD of stability was less than 10.7% at 4°C for 48 h. The 144 Adulterated Products obtained over 3 years (2014–2016) from online and in-person vendors were tested using established methods. After rapidly screening with Quadrupole-Orbitrap mass spectrometry, the detected samples were quantified using ultra high performance liquid chromatography with tandem mass spectrometry. Two of them were Adulterated with phenobarbital. This article is protected by copyright. All rights reserved
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A Liquid Chromatography‐Quadrupole‐Time of Flight Mass Spectrometry (LC‐Q‐TOF MS) Study for Analyzing 35 Corticosteroid Compounds: Elucidation of MS/MS Fragmentation Pathways
Bulletin of The Korean Chemical Society, 2016Co-Authors: Chang-yong Yoon, Sun Young Baek, Jung-ah DoAbstract:Corticosteroids have been often found to be added to a dietary supplement for the purpose of illegally improving the effect of their Products. Thus, it is imperative to develop or improve a method that enables one to rapidly and reliably analyze corticosteroids in health or dietary supplements, for the safety management purpose. In the present study, results from liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS) experiments for the selected 35 corticosteroid compounds are presented, which can be useful for the qualitative screening of corticosteroids in health or dietary supplements. Specifically, retention times, accurate mass data of the protonated steroids, m/z values of major fragment ions are given for the 35 corticosteroids. Further, fragmentation pathways for the selected steroids are also suggested. Based on the suggested fragmentation pathways, it was shown that an unknown steroid compound can be readily identified using the knowledge of a group of unique and specific common skeletal fragments. The high selectivity and sensitivity of the LC-Q-TOF-MS/MS results combined with the knowledge of the fragmentation pathways can offer a new opportunity for rapid and accurate screening of corticosteroids, thus preventing health-related incidents involving Adulterated Products and clamping down on illegally circulated health Products.
Han Na Park - One of the best experts on this subject based on the ideXlab platform.
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development of a specific fragment pattern based quadrupole orbitrap mass spectrometry method to screen Adulterated Products of phosphodiesterase 5 inhibitors and their analogues
Science & Justice, 2019Co-Authors: Han Na Park, Seong Soo Park, Hoil KangAbstract:Abstract Recently, Adulterated supplements with phosphodiesterase-5 inhibitors (PDE-5i) have frequently observed. New synthetic analogues obtained from the chemical modification of parent compounds are frequently found in illicit Products despite continuous efforts to inspect for these adulterants. A rapid and accurate method based on quadrupole-Orbitrap mass spectrometry was developed for simultaneously confirming and quantifying 85 PDE-5i and derived analogues present in illicit Products for erectile dysfunction (ED). Common ions of PDE-5i according to their similar structures were proposed based on MS/MS fragmentations. These common ions could be an important diagnosis of their presence targets or new emerging analogues in supplements. Several validation parameters were employed, resulting in a limit of detection and quantification of 0.09–8.55 ng/mL and 0.24–17.10 ng/mL, respectively. The linear correlation coefficient ( r 2 ) was higher than 0.995, and mean recoveries of target compounds were in the range of 82–118%. A total of 187 illicit Products, obtained from on/offline markets over a period of 3 years (2015–2017), were screened by the established method. Approximately 53% of them were Adulterated with PDE-5i or derived analogues at concentrations of 0.1–726.0 mg/g in the illicit Products. In the interests of public health, this study describes a rapid and accurate method to determine PDE-5i and new emerging analogues in Adulterated Products.
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development and validation of rapid and simultaneous method for determination of 12 hair growth compounds in Adulterated Products by uhplc ms ms
Forensic Science International, 2018Co-Authors: Han Na Park, Sun Young Baek, Sungkwan Park, Hoil KangAbstract:Abstract Synthetic hair-growth compounds have been illegally used in diverse Products to enhance the short-term efficacy of these Products. In this study, a rapid and simultaneous method for the determination of hair-growth compounds in Adulterated Products based on ultra high pressure liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) was developed and validated. The limit of detection (LOD) and limit of quantitation (LOQs) of the method were 0.08–43.6 ng/mL and 0.27–145 ng/mL for the solid-, liquid-, and cream-type samples, respectively. Good calibration linearity for all compounds was demonstrated with a correlation coefficient (r2) higher than 0.997. The intra- and inter-assay precisions were within 11%. The corresponding accuracies were 86–117% and 81–113%, respectively. The mean recoveries obtained for the solid-, liquid, and cream-type samples ranged from 87 to 114%, with a relative standard deviation (RSD) within 6%. The RSD of the stability evaluated at 4 °C for 48 h was less than 6%. The established method was used to screen 76 samples advertised as hair-growth treatments, from online and offline markets, over the course of two years. In 10% of the samples, four compounds, including triaminodil, minoxidil, finasteride, methyltestosterone, and testosterone–propionate were detected. The concentrations were in the range of 0.5–16.4 mg/g. This technique provides a reliable platform for technical analysis for continuous monitoring of Adulterated Products to protect public health.
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simultaneous analysis by quadrupole orbitrap mass spectrometry and uhplc ms ms for the determination of sedative hypnotics and sleep inducers in Adulterated Products
IEEE Journal of Solid-state Circuits, 2017Co-Authors: Han Na Park, Ji Yeon Choi, Hyungjoon Park, Seong Soo Park, Sun Young BaekAbstract:Adulterated Products are continuously detected in society and cause problems. In this study, we developed and validated a method for determining synthetic sedative-hypnotics and sleep inducers, including barbital, benzodiazepam, zolpidem, and first-generation antihistamines, in Adulterated Products using Quadrupole-Orbitrap mass spectrometry and ultrahigh performance liquid chromatography with tandem mass spectrometry. In Quadrupole-Orbitrap mass spectrometry analysis, target compounds were confirmed using a combination of retention time, mass tolerance, mass accuracy, and fragment ions. For quantification, several validation parameters were employed using ultrahigh performance liquid chromatography with tandem mass spectrometry. The limit of detection and limit of quantitation was 0.05-53 and 0.17-177 ng/mL, respectively. The correlation coefficient for linearity was more than 0.995. The intra- and interassay accuracies were 86-110 and 84-111%, respectively. Their precision values were evaluated as within 4.0 (intraday) and 10.7% (interday). Mean recoveries of target compounds in Adulterated Products ranged from 85 to 116%. The relative standard deviation of stability was less than 10.7% at 4°C for 48 h. The 144 Adulterated Products obtained over 3 years (2014-2016) from online and in-person vendors were tested using established methods. After rapidly screening with Quadrupole-Orbitrap mass spectrometry, the detected samples were quantified using ultrahigh performance liquid chromatography with tandem mass spectrometry. Two of them were Adulterated with phenobarbital.
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Simultaneous analysis by Quadrupole‐Orbitrap mass spectrometry and UHPLC‐MS/MS for the determination of sedative‐hypnotics and sleep inducers in Adulterated Products
Journal of Separation Science, 2017Co-Authors: Han Na Park, Ji Yeon Choi, Hyungjoon Park, Seong Soo Park, Sun Young BaekAbstract:Adulterated Products are continuously detected in society and cause problems. In this study, we developed and validated a method for determining synthetic sedative-hypnotics and sleep inducers, including barbital, benzodiazepam, zolpidem, and first-generation antihistamines, in Adulterated Products using Quadrupole-Orbitrap mass spectrometry and ultra high performance liquid chromatography with tandem mass spectrometry. In Quadrupole-Orbitrap mass spectrometry analysis, target compounds were confirmed using a combination of retention time, mass tolerance, mass accuracy, and fragment ions. For quantification, several validation parameters were employed using ultra high performance liquid chromatography with tandem mass spectrometry. The limit of detection and limit of quantitation was 0.05–53 and 0.17–177 ng/mL, respectively. The correlation coefficient for linearity was more than 0.995. The intra- and inter-assay accuracies were 86–110 and 84–111%, respectively. Their precision values were evaluated as within 4.0 (intra-day) and 10.7% (inter-day). Mean recoveries of target compounds in Adulterated Products ranged from 85 to 116%. The relative SD of stability was less than 10.7% at 4°C for 48 h. The 144 Adulterated Products obtained over 3 years (2014–2016) from online and in-person vendors were tested using established methods. After rapidly screening with Quadrupole-Orbitrap mass spectrometry, the detected samples were quantified using ultra high performance liquid chromatography with tandem mass spectrometry. Two of them were Adulterated with phenobarbital. This article is protected by copyright. All rights reserved
Panagiotis Madesis - One of the best experts on this subject based on the ideXlab platform.
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Hybrid analysis (barcode-high resolution melting) for authentication of Thai herbal Products, Andrographis paniculata (Burm.f.) Wall.ex Nees
Pharmacognosy Magazine, 2020Co-Authors: Maslin Osathanunkul, C. Suwannapoom, Nuttaluck Khamyong, Danupol Pintakum, Santisuk Na Lamphun, Kanokporn Triwitayakorn, Kitisak Osathanunkul, Panagiotis MadesisAbstract:Background: Andrographis paniculata Nees is a medicinal plant with multiple pharmacological properties. It has been used over many centuries as a household remedy. A. paniculata Products sold on the markets are in processed forms so it is difficult to authenticate. Therefore buying the herbal Products poses a high-risk of acquiring counterfeited, substituted and/or Adulterated Products. Due to these issues, a reliable method to authenticate Products is needed. Materials and Methods: High resolution melting analysis coupled with DNA barcoding (Bar-HRM) was applied to detect adulteration in commercial herbal Products. The rbc L barcode was selected to use in primers design for HRM analysis to produce standard melting profile of A. paniculata species. DNA of the tested commercial Products was isolated and their melting profiles were then generated and compared with the standard A. paniculata . Results: The melting profiles of the rbc L amplicons of the three closely related herbal species ( A. paniculata , Acanthus ebracteatus and Rhinacanthus nasutus ) are clearly separated so that they can be distinguished by the developed method. The method was then used to authenticate commercial herbal Products. HRM curves of all 10 samples tested are similar to A. paniculata which indicated that all tested Products were contained the correct species as labeled. Conclusion: The method described in this study has been proved to be useful in aiding identification and/or authenticating A. paniculata . This Bar-HRM analysis has allowed us easily to determine the A. paniculata species in herbal Products on the markets even they are in processed forms.
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Hybrid analysis (barcode-high resolution melting) for authentication of Thai herbal Products, Andrographis paniculata (Burm.f.) Wall.ex Nees.
Pharmacognosy magazine, 2020Co-Authors: Maslin Osathanunkul, C. Suwannapoom, Nuttaluck Khamyong, Danupol Pintakum, Santisuk Na Lamphun, Kanokporn Triwitayakorn, Kitisak Osathanunkul, Panagiotis MadesisAbstract:Andrographis paniculata Nees is a medicinal plant with multiple pharmacological properties. It has been used over many centuries as a household remedy. A. paniculata Products sold on the markets are in processed forms so it is difficult to authenticate. Therefore buying the herbal Products poses a high-risk of acquiring counterfeited, substituted and/or Adulterated Products. Due to these issues, a reliable method to authenticate Products is needed. High resolution melting analysis coupled with DNA barcoding (Bar-HRM) was applied to detect adulteration in commercial herbal Products. The rbcL barcode was selected to use in primers design for HRM analysis to produce standard melting profile of A. paniculata species. DNA of the tested commercial Products was isolated and their melting profiles were then generated and compared with the standard A. paniculata. The melting profiles of the rbcL amplicons of the three closely related herbal species (A. paniculata, Acanthus ebracteatus and Rhinacanthus nasutus) are clearly separated so that they can be distinguished by the developed method. The method was then used to authenticate commercial herbal Products. HRM curves of all 10 samples tested are similar to A. paniculata which indicated that all tested Products were contained the correct species as labeled. The method described in this study has been proved to be useful in aiding identification and/or authenticating A. paniculata. This Bar-HRM analysis has allowed us easily to determine the A. paniculata species in herbal Products on the markets even they are in processed forms. We propose the use of DNA barcoding combined with High Resolution Melting analysis for authenticating of Andrographis paniculata Products.The developed method can be used regardless of the type of the DNA template (fresh or dried tissue, leaf, and stem).rbcL region was chosen for the analysis and work well with our samplesWe can easily determine the A. paniculata species in herbal Products tested. Abbreviations used: bp: Base pair, Tm: Melting temperature.
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Bar-HRM for authentication of plant-based medicines: Evaluation of three medicinal Products derived from Acanthaceae species
PLOS ONE, 2015Co-Authors: Maslin Osathanunkul, Panagiotis Madesis, Hugo J. De BoerAbstract:Medicinal plants are used as a popular alternative to synthetic drugs, both in developed and developing countries. The economic importance of the herbal and natural supplement industry is increasing every year. As the herbal industry grows, consumer safety is one issue that cannot be overlooked. Herbal Products in Thai local markets are commonly sold without packaging or labels. Plant powders are stored in large bags or boxes, and therefore buying local herbal Products poses a high risk of acquiring counterfeited, substituted and/or Adulterated Products. Due to these issues, a reliable method to authenticate Products is needed. Here DNA barcoding was used in combination with High Resolution Melting analysis (Bar-HRM) to authenticate three medicinal Acanthaceae species (Acanthus ebracteatus, Andrographis paniculata and Rhinacanthus nasutus) commonly used in Thailand. The rbcL barcode was selected for use in primers design for HRM analysis to produce standard melting profiles of the selected species. Melting data from the HRM assay using the designed rbcL primers showed that the three chosen species could be distinguished from each other. HRM curves of all fifteen test samples indicated that three of tested Products did not contain the indicated species. Two closely related species (A. paniculata and R. nasutus), which have a high level of morphological similarity, were interchanged with one another in three tested Products. Incorrect information on packaging and labels of the tested herbal Products was the cause of the results shown here. Morphological similarity among the species of interest also hindered the collection process. The Bar-HRM method developed here proved useful in aiding in the identification and authentication of herbal species in processed samples. In the future, species authentication through Bar-HRM could be used to promote consumer trust, as well as raising the quality of herbal Products.
Maslin Osathanunkul - One of the best experts on this subject based on the ideXlab platform.
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Hybrid analysis (barcode-high resolution melting) for authentication of Thai herbal Products, Andrographis paniculata (Burm.f.) Wall.ex Nees
Pharmacognosy Magazine, 2020Co-Authors: Maslin Osathanunkul, C. Suwannapoom, Nuttaluck Khamyong, Danupol Pintakum, Santisuk Na Lamphun, Kanokporn Triwitayakorn, Kitisak Osathanunkul, Panagiotis MadesisAbstract:Background: Andrographis paniculata Nees is a medicinal plant with multiple pharmacological properties. It has been used over many centuries as a household remedy. A. paniculata Products sold on the markets are in processed forms so it is difficult to authenticate. Therefore buying the herbal Products poses a high-risk of acquiring counterfeited, substituted and/or Adulterated Products. Due to these issues, a reliable method to authenticate Products is needed. Materials and Methods: High resolution melting analysis coupled with DNA barcoding (Bar-HRM) was applied to detect adulteration in commercial herbal Products. The rbc L barcode was selected to use in primers design for HRM analysis to produce standard melting profile of A. paniculata species. DNA of the tested commercial Products was isolated and their melting profiles were then generated and compared with the standard A. paniculata . Results: The melting profiles of the rbc L amplicons of the three closely related herbal species ( A. paniculata , Acanthus ebracteatus and Rhinacanthus nasutus ) are clearly separated so that they can be distinguished by the developed method. The method was then used to authenticate commercial herbal Products. HRM curves of all 10 samples tested are similar to A. paniculata which indicated that all tested Products were contained the correct species as labeled. Conclusion: The method described in this study has been proved to be useful in aiding identification and/or authenticating A. paniculata . This Bar-HRM analysis has allowed us easily to determine the A. paniculata species in herbal Products on the markets even they are in processed forms.
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Hybrid analysis (barcode-high resolution melting) for authentication of Thai herbal Products, Andrographis paniculata (Burm.f.) Wall.ex Nees.
Pharmacognosy magazine, 2020Co-Authors: Maslin Osathanunkul, C. Suwannapoom, Nuttaluck Khamyong, Danupol Pintakum, Santisuk Na Lamphun, Kanokporn Triwitayakorn, Kitisak Osathanunkul, Panagiotis MadesisAbstract:Andrographis paniculata Nees is a medicinal plant with multiple pharmacological properties. It has been used over many centuries as a household remedy. A. paniculata Products sold on the markets are in processed forms so it is difficult to authenticate. Therefore buying the herbal Products poses a high-risk of acquiring counterfeited, substituted and/or Adulterated Products. Due to these issues, a reliable method to authenticate Products is needed. High resolution melting analysis coupled with DNA barcoding (Bar-HRM) was applied to detect adulteration in commercial herbal Products. The rbcL barcode was selected to use in primers design for HRM analysis to produce standard melting profile of A. paniculata species. DNA of the tested commercial Products was isolated and their melting profiles were then generated and compared with the standard A. paniculata. The melting profiles of the rbcL amplicons of the three closely related herbal species (A. paniculata, Acanthus ebracteatus and Rhinacanthus nasutus) are clearly separated so that they can be distinguished by the developed method. The method was then used to authenticate commercial herbal Products. HRM curves of all 10 samples tested are similar to A. paniculata which indicated that all tested Products were contained the correct species as labeled. The method described in this study has been proved to be useful in aiding identification and/or authenticating A. paniculata. This Bar-HRM analysis has allowed us easily to determine the A. paniculata species in herbal Products on the markets even they are in processed forms. We propose the use of DNA barcoding combined with High Resolution Melting analysis for authenticating of Andrographis paniculata Products.The developed method can be used regardless of the type of the DNA template (fresh or dried tissue, leaf, and stem).rbcL region was chosen for the analysis and work well with our samplesWe can easily determine the A. paniculata species in herbal Products tested. Abbreviations used: bp: Base pair, Tm: Melting temperature.
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Bar-HRM for authentication of plant-based medicines: Evaluation of three medicinal Products derived from Acanthaceae species
PLOS ONE, 2015Co-Authors: Maslin Osathanunkul, Panagiotis Madesis, Hugo J. De BoerAbstract:Medicinal plants are used as a popular alternative to synthetic drugs, both in developed and developing countries. The economic importance of the herbal and natural supplement industry is increasing every year. As the herbal industry grows, consumer safety is one issue that cannot be overlooked. Herbal Products in Thai local markets are commonly sold without packaging or labels. Plant powders are stored in large bags or boxes, and therefore buying local herbal Products poses a high risk of acquiring counterfeited, substituted and/or Adulterated Products. Due to these issues, a reliable method to authenticate Products is needed. Here DNA barcoding was used in combination with High Resolution Melting analysis (Bar-HRM) to authenticate three medicinal Acanthaceae species (Acanthus ebracteatus, Andrographis paniculata and Rhinacanthus nasutus) commonly used in Thailand. The rbcL barcode was selected for use in primers design for HRM analysis to produce standard melting profiles of the selected species. Melting data from the HRM assay using the designed rbcL primers showed that the three chosen species could be distinguished from each other. HRM curves of all fifteen test samples indicated that three of tested Products did not contain the indicated species. Two closely related species (A. paniculata and R. nasutus), which have a high level of morphological similarity, were interchanged with one another in three tested Products. Incorrect information on packaging and labels of the tested herbal Products was the cause of the results shown here. Morphological similarity among the species of interest also hindered the collection process. The Bar-HRM method developed here proved useful in aiding in the identification and authentication of herbal species in processed samples. In the future, species authentication through Bar-HRM could be used to promote consumer trust, as well as raising the quality of herbal Products.
Hoil Kang - One of the best experts on this subject based on the ideXlab platform.
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development of a specific fragment pattern based quadrupole orbitrap mass spectrometry method to screen Adulterated Products of phosphodiesterase 5 inhibitors and their analogues
Science & Justice, 2019Co-Authors: Han Na Park, Seong Soo Park, Hoil KangAbstract:Abstract Recently, Adulterated supplements with phosphodiesterase-5 inhibitors (PDE-5i) have frequently observed. New synthetic analogues obtained from the chemical modification of parent compounds are frequently found in illicit Products despite continuous efforts to inspect for these adulterants. A rapid and accurate method based on quadrupole-Orbitrap mass spectrometry was developed for simultaneously confirming and quantifying 85 PDE-5i and derived analogues present in illicit Products for erectile dysfunction (ED). Common ions of PDE-5i according to their similar structures were proposed based on MS/MS fragmentations. These common ions could be an important diagnosis of their presence targets or new emerging analogues in supplements. Several validation parameters were employed, resulting in a limit of detection and quantification of 0.09–8.55 ng/mL and 0.24–17.10 ng/mL, respectively. The linear correlation coefficient ( r 2 ) was higher than 0.995, and mean recoveries of target compounds were in the range of 82–118%. A total of 187 illicit Products, obtained from on/offline markets over a period of 3 years (2015–2017), were screened by the established method. Approximately 53% of them were Adulterated with PDE-5i or derived analogues at concentrations of 0.1–726.0 mg/g in the illicit Products. In the interests of public health, this study describes a rapid and accurate method to determine PDE-5i and new emerging analogues in Adulterated Products.
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development and validation of rapid and simultaneous method for determination of 12 hair growth compounds in Adulterated Products by uhplc ms ms
Forensic Science International, 2018Co-Authors: Han Na Park, Sun Young Baek, Sungkwan Park, Hoil KangAbstract:Abstract Synthetic hair-growth compounds have been illegally used in diverse Products to enhance the short-term efficacy of these Products. In this study, a rapid and simultaneous method for the determination of hair-growth compounds in Adulterated Products based on ultra high pressure liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) was developed and validated. The limit of detection (LOD) and limit of quantitation (LOQs) of the method were 0.08–43.6 ng/mL and 0.27–145 ng/mL for the solid-, liquid-, and cream-type samples, respectively. Good calibration linearity for all compounds was demonstrated with a correlation coefficient (r2) higher than 0.997. The intra- and inter-assay precisions were within 11%. The corresponding accuracies were 86–117% and 81–113%, respectively. The mean recoveries obtained for the solid-, liquid, and cream-type samples ranged from 87 to 114%, with a relative standard deviation (RSD) within 6%. The RSD of the stability evaluated at 4 °C for 48 h was less than 6%. The established method was used to screen 76 samples advertised as hair-growth treatments, from online and offline markets, over the course of two years. In 10% of the samples, four compounds, including triaminodil, minoxidil, finasteride, methyltestosterone, and testosterone–propionate were detected. The concentrations were in the range of 0.5–16.4 mg/g. This technique provides a reliable platform for technical analysis for continuous monitoring of Adulterated Products to protect public health.
