Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software

In recent years, the illegal addition of male sexual function-regulating compounds in traditional Chinese medicine (TCM) has attracted widespread attention. These illegally added compounds may have specific pharmacological and toxic side effects, which can endanger lives when taken with other relate...

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Main Authors: Min LIAO, Ying-chao WANG, Qi CHEN, Lian JIANG, Hai-ning WANG
Format: Article
Language:English
Published: Editorial Board of Journal of Chinese Mass Spectrometry Society 2025-05-01
Series:Zhipu Xuebao
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Online Access:https://zpxb.xml-journal.net/article/doi/10.7538/zpxb.2024.0134
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author Min LIAO
Ying-chao WANG
Qi CHEN
Lian JIANG
Hai-ning WANG
author_facet Min LIAO
Ying-chao WANG
Qi CHEN
Lian JIANG
Hai-ning WANG
author_sort Min LIAO
collection DOAJ
description In recent years, the illegal addition of male sexual function-regulating compounds in traditional Chinese medicine (TCM) has attracted widespread attention. These illegally added compounds may have specific pharmacological and toxic side effects, which can endanger lives when taken with other related therapeutic drugs. In 2009, National Medical Products Administration of China established a standard detection method for illegal sexual function-regulating compounds in TCM. However, this method has limits of long detection time, low qualitative accuracy, and narrow detection range, making it inadequate for regulatory requirements. In this study, a method of ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF MS) combined with UNIFI software was developed for detecting illegally added compounds used to treat premature ejaculation (PE) and erectile dysfunction (ED) in TCM. Sample preparation methods were selected according to different TCM formulations. Chromatographic separation was performed on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm). The mobile phase consisted of acetonitrile-0.1% formic acid solution with gradient elution at a column temperature of 30 ℃. Data acquisition was conducted in MSE mode under positive electrospray ionization with a mass scan range of m/z 50-1 200. A targeted screening database for illegal additives was constructed in UNIFI software based on chromatographic retention time, precise mass of parent ions and fragment ions of reference standards. Screening conditions were set according to EU SANTE/11312/2021 guidelines, and automated screening and analysis of detection results were achieved through the UNIFI software. Compared with the standard detection method, this method reduces the detection time from 160 min to 12 min, and expands the detection range from 11 ED treatment compounds to 31 compounds, including 11 new ED-treating compounds and 9 PE-treating compounds. The limits of detection are 0.25 to 15.00 mg/kg (or mg/L). In the detection of 20 batches of kidney-tonifying and yang-strengthening TCM samples, illegal additions are found in 7 batches, with 4 batches containing compounds beyond the scope of the standard detection method. This method has advantages of rapid detection, high accuracy, broad detection range, and flexible expansion capability, which can provide more robust technical support for regulatory oversight of illegal additions in TCM.
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language English
publishDate 2025-05-01
publisher Editorial Board of Journal of Chinese Mass Spectrometry Society
record_format Article
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spelling doaj-art-2d818e71e23d4c80b67912cb5b47b4e72025-08-20T03:48:10ZengEditorial Board of Journal of Chinese Mass Spectrometry SocietyZhipu Xuebao1004-29972025-05-0146337037910.7538/zpxb.2024.01342024-134-d9Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI SoftwareMin LIAO0Ying-chao WANG1Qi CHEN2Lian JIANG3Hai-ning WANG4Guizhou Institute for Food and Drug Control, Guiyang 550081, ChinaGuizhou Institute for Food and Drug Control, Guiyang 550081, ChinaGuizhou Institute for Food and Drug Control, Guiyang 550081, ChinaGuizhou Institute for Food and Drug Control, Guiyang 550081, ChinaGuizhou Institute for Food and Drug Control, Guiyang 550081, ChinaIn recent years, the illegal addition of male sexual function-regulating compounds in traditional Chinese medicine (TCM) has attracted widespread attention. These illegally added compounds may have specific pharmacological and toxic side effects, which can endanger lives when taken with other related therapeutic drugs. In 2009, National Medical Products Administration of China established a standard detection method for illegal sexual function-regulating compounds in TCM. However, this method has limits of long detection time, low qualitative accuracy, and narrow detection range, making it inadequate for regulatory requirements. In this study, a method of ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF MS) combined with UNIFI software was developed for detecting illegally added compounds used to treat premature ejaculation (PE) and erectile dysfunction (ED) in TCM. Sample preparation methods were selected according to different TCM formulations. Chromatographic separation was performed on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm). The mobile phase consisted of acetonitrile-0.1% formic acid solution with gradient elution at a column temperature of 30 ℃. Data acquisition was conducted in MSE mode under positive electrospray ionization with a mass scan range of m/z 50-1 200. A targeted screening database for illegal additives was constructed in UNIFI software based on chromatographic retention time, precise mass of parent ions and fragment ions of reference standards. Screening conditions were set according to EU SANTE/11312/2021 guidelines, and automated screening and analysis of detection results were achieved through the UNIFI software. Compared with the standard detection method, this method reduces the detection time from 160 min to 12 min, and expands the detection range from 11 ED treatment compounds to 31 compounds, including 11 new ED-treating compounds and 9 PE-treating compounds. The limits of detection are 0.25 to 15.00 mg/kg (or mg/L). In the detection of 20 batches of kidney-tonifying and yang-strengthening TCM samples, illegal additions are found in 7 batches, with 4 batches containing compounds beyond the scope of the standard detection method. This method has advantages of rapid detection, high accuracy, broad detection range, and flexible expansion capability, which can provide more robust technical support for regulatory oversight of illegal additions in TCM.https://zpxb.xml-journal.net/article/doi/10.7538/zpxb.2024.0134ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (uplc-q-tof ms)unifi softwaretraditional chinese medicineillegal additioncompounds regulating sexual functionrapid screening
spellingShingle Min LIAO
Ying-chao WANG
Qi CHEN
Lian JIANG
Hai-ning WANG
Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software
Zhipu Xuebao
ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (uplc-q-tof ms)
unifi software
traditional chinese medicine
illegal addition
compounds regulating sexual function
rapid screening
title Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software
title_full Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software
title_fullStr Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software
title_full_unstemmed Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software
title_short Rapid Screening of Illegal Addition of Compounds Regulating Sexual Function in Traditional Chinese Medicine Based on UPLC-Q-TOF MS Technique Combined with UNIFI Software
title_sort rapid screening of illegal addition of compounds regulating sexual function in traditional chinese medicine based on uplc q tof ms technique combined with unifi software
topic ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (uplc-q-tof ms)
unifi software
traditional chinese medicine
illegal addition
compounds regulating sexual function
rapid screening
url https://zpxb.xml-journal.net/article/doi/10.7538/zpxb.2024.0134
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