Characterization of a new component and impurities in josamycin by trap‐free two‐dimensional liquid chromatography coupled to ion trap time‐of‐flight mass spectrometry

Liu, Guijun; Yu, Xu; Sang, Jing; Zhu, Bingqi; Wang, Jian

doi:10.1002/rcm.8439

Cited by 13 publications

(2 citation statements)

References 27 publications

(50 reference statements)

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“…Because of the complexity of these components, their comprehensive analysis was extremely difficult. Since the mid‐2000s, because of its high separation resolution, enhanced separation speed, unmatched sensitivity, and minimal sample preparation, liquid chromatography/mass spectrometry (LC/MS) has been increasingly used in natural products research . In addition, the low sample quantity requirement makes LC/MS even more attractive to TCM scientists.…”

Section: Introductionmentioning

confidence: 99%

Structural characterization and discrimination of Paris polyphylla var. yunnanensis by a molecular networking strategy coupled with ultra‐high‐performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry

Wang

Fan

Xiang

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale: Paris polyphylla var. yunnanensis (Franch) Hand Mazz (PPY) is a traditionalChinese medicine with antitumor, antibacterial, hemostatic, and anthelmintic activities. Identification of the chemical composition in PPY is helpful to discover its active ingredients and can be used to establish its quality control protocols.Methods: The composition of PPY was identified using ultra-high-performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry (UHPLC/QTOF-MS/MS) coupled with a molecular networking strategy. First, the UHPLC/QTOF-MS/MS approach was optimized for chemical compound profiling.Then, the MS data were processed using PeakView™ combined with an in-house database to quickly characterize the secondary metabolites. Finally, molecular networking excavated new molecular weights to discover unknown or trace natural products based on the characteristics of each cluster. Results:A total of 222 compounds, including 77 isospirostanols, 2 spirostanols, 19 furostanols, 10 pseudospirostanols, 6 cholesterols, 10 C 21 steroids, 5 insect metamorphosis hormones, 3 plant sterols, 6 five-ring triterpenoids, 4 flavonoids, 8 fatty acids, 2 phenylpropanoids, and 8 other compounds, were characterized in PPY by comparing their main fragmentation characteristics and pathways with the literature data, and 62 of them, 54 steroidals and 8 phenylpropanoids, were discovered or tentatively identified for the first time. Conclusions:This study extended the application of a molecular networking strategy to traditional herbal medicines and developed a molecular networking based screening approach with a significant increase in efficiency for the discovery and identification of trace novel natural products.Yumei Wang and Qian Fan contributed equally to this work as first authors. Paris polyphylla var. yunnanensis (Franch) Hand Mazz (PPY), calledChong Lou, is a well-known, valuable traditional Chinese medicine (TCM) that has been used to treat fractures, hemorrhages, snake bites, and abscess for many years. 1,2 PPY has been used as a main ingredient for the preparation of many TCMs, such as Yunnan Baiyao, Gongxuening capsules, and Jidesheng Sheyao tablets. 3 Phytochemistry studies have indicated that the dried rhizomes of Paris species contain steroidal saponins, triterpenoid saponins, flavonoids, phenylpropanoids, ecdysteroids, phenolic glycosides, and so on. 4-6 The glucosyl groups of steroidal saponins are normally attached to the steroidal aglycones through the hydroxyl groups at the C-3 and/or C-26 positions (and sometimes the C-1, C-21, C-23, and C-24 positions). Four types of steroidal sapogenins 6 (spirostanol, isospirostanol, furostanol, and pseudospirostanol) are considered major aglycones, and typical sugars are arabinose, xylose, apiose, fucose, rhamnose, glucose, and galactose. Comprehensive identification of ingredients in PPY is critical to understanding its biological mechanism and establishing quality control protocols. Because of the complexity of these components, their comprehensive...

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Section: Introductionmentioning

confidence: 99%

Structural characterization and discrimination of Paris polyphylla var. yunnanensis by a molecular networking strategy coupled with ultra‐high‐performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry

Wang

Fan

Xiang

et al. 2020

Rapid Comm Mass Spectrometry

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“…More and more structural information can be obtained using liquid chromatography tandem mass spectrometry (LC–MS n ) analysis, which shows great superiority to identify the impurities 4–8 . The impurities in actinomycins were identified and reported using LC‐MS 9–13 …”

Section: Introductionmentioning

confidence: 99%

Separation and characterization of two series of unknown degradation impurities caused by light irradiation and autoclaving in xinfujunsu injection using liquid chromatography tandem mass spectrometry

Qiaoqiao

Tang

Ren

et al. 2021

Rapid Comm Mass Spectrometry

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Rationale A series of photodegradation impurities and a series of degradation impurities produced in autoclaving in xinfujunsu injection were discovered, and these unknown impurities were separated and characterized thoroughly using liquid chromatography tandem quadrupole time‐of‐flight mass spectrometry. Methods The column was a Platisil 5 μm ODS (4.6 × 250 mm, 5 μm). For the analysis of degradation impurities caused by light irradiation and autoclaving, the mobile phase was composed of 0.01 M ammonium formate aqueous solution and acetonitrile/isopropanol (90:10, V/V). Full scan LC–MS and LC–MS2 was carried out to obtain as much structural information as possible. The fragmentation behavior of actinomycin D, actinomycin S3, and its impurities was studied and used to obtain information about the structures of these impurities. Results Based on MS2 spectral data and exact mass measurements, the chemical structures of two series of degradation impurities were characterized, among which five unknown impurities were photodegradation impurities and seven unknown impurities were degradation impurities produced in autoclaving of xinfujunsu injection. Conclusions Based on characterization of impurities, this study also revealed the cause of impurity production and provided guidance for enterprises to improve the process and drug packaging material to reduce impurity content. Furthermore, this study also provided scientific basis for further improvement of official monographs in pharmacopoeias.

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Advances of hyphenated technique in impurity profiling of active pharmaceutical ingredients and pharmaceutical products

Khandale,

Rajge,

Singh

et al. 2023

Separation Science Plus

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Impurities found in active pharmaceutical ingredients (APIs) and pharmaceutical products are of ever‐increasing interest. According to several regulatory agencies, purity and impurity profiles are essential. An impurity is defined as any additional inorganic or organic material, residual solvents other than the medicinal components, or undesired compounds that remain with APIs. Impurities and degradation products in bulk drug materials and pharmaceutical formulations are identified, their structures are clarified, and their quantitative determination is part of impurity profiling. Unrecognized, poisonous impurities are dangerous to health and should be identified by selective procedures to increase the safety of drug therapy, and impurity profiling has become more significant in pharmaceutical analysis. This review briefly introduces process and product‐related impurities and emphasizes the creation of cutting‐edge analytical techniques for identifying them. It discusses the use of analytical methods, particularly high‐performance thin‐layer chromatography, liquid chromatography with mass spectrometry (MS), ultrahigh‐performance liquid chromatography, gas chromatography–MS, and nuclear magnetic resonance spectroscopy for the identification of contaminants and degradation products. It has discussed the importance of the quality, efficacy, and safety of drug substances and products, including the origin, types, and quality control of impurities, the need for the development of impurity profiling methods, impurity identification, and regulatory aspects.

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Characterization of a new component and impurities in josamycin by trap‐free two‐dimensional liquid chromatography coupled to ion trap time‐of‐flight mass spectrometry

Cited by 13 publications

References 27 publications

Structural characterization and discrimination of Paris polyphylla var. yunnanensis by a molecular networking strategy coupled with ultra‐high‐performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry

Structural characterization and discrimination of Paris polyphylla var. yunnanensis by a molecular networking strategy coupled with ultra‐high‐performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry

Separation and characterization of two series of unknown degradation impurities caused by light irradiation and autoclaving in xinfujunsu injection using liquid chromatography tandem mass spectrometry

Advances of hyphenated technique in impurity profiling of active pharmaceutical ingredients and pharmaceutical products

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