A high‐performance liquid chromatography‐tandem mass spectrometry method has been developed for the determination of irinotecan, 7‐ethyl‐10‐hydroxycamptothecin (SN38), and SN38 glucuronide (SN38G) in rat plasma in the present study. The analytes were separated on a C18 column and a triple‐quadrupole mass spectrometry equipped with an electrospray ionization source was applied for detection. Irinotecan, SN38 and SN38G could be well retained in the C18 column after optimization of mobile phase. A simple protein precipitation was used to pretreat the plasma. The extraction recovery was above 90% and the matrix effect could be negligible. The method was linear over the concentration ranges of 3.46–3458.8 ng/mL for irinotecan, 2.53–2530.0 ng/mL for SN38 and 2.5–2500.0 ng/mL for SN38G. The precision and accuracy was within the acceptable limits. The simple and convenient method was validated and successfully applied to support the pharmacokinetic study and elucidate the mechanism of irinotecan‐induced diarrhea after irinotecan was intravenously injected to the Sprague‐Dawley rats.
{"title":"A validated high‐performance liquid chromatography‐tandem mass spectrometry method for simultaneous determination of irinotecan and two major metabolites in rat plasma: Application for the pharmacokinetics study","authors":"Liangzhu Jiang, Gu Nan, Peng Yuzhi, Liao Yuxin, Zhou Limin, Yongbing Sun","doi":"10.1002/sscp.202400069","DOIUrl":"https://doi.org/10.1002/sscp.202400069","url":null,"abstract":"A high‐performance liquid chromatography‐tandem mass spectrometry method has been developed for the determination of irinotecan, 7‐ethyl‐10‐hydroxycamptothecin (SN38), and SN38 glucuronide (SN38G) in rat plasma in the present study. The analytes were separated on a C18 column and a triple‐quadrupole mass spectrometry equipped with an electrospray ionization source was applied for detection. Irinotecan, SN38 and SN38G could be well retained in the C18 column after optimization of mobile phase. A simple protein precipitation was used to pretreat the plasma. The extraction recovery was above 90% and the matrix effect could be negligible. The method was linear over the concentration ranges of 3.46–3458.8 ng/mL for irinotecan, 2.53–2530.0 ng/mL for SN38 and 2.5–2500.0 ng/mL for SN38G. The precision and accuracy was within the acceptable limits. The simple and convenient method was validated and successfully applied to support the pharmacokinetic study and elucidate the mechanism of irinotecan‐induced diarrhea after irinotecan was intravenously injected to the Sprague‐Dawley rats.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140992737","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Sulfonate esters are a class of organic impurities that includes highly potent mutagenic substances that typically need to be controlled down to a low ppm level in pharmaceutical development. In this work, two genotoxic impurities of sulfonate esters in Posaconazole, for example, ((3S,5R)‐5‐((1H‐1,2,4‐triazol‐1‐yl)methyl)‐5‐(2,4‐difluorophenyl)tetrahydrofuran‐3‐yl)methyl‐4‐methylbenzenesulfonate and (2S,3S)‐3‐ (4‐(4‐(4‐(4‐(((3R,5R)‐5‐((1H‐1,2,4‐triazol‐1‐yl)methyl)‐5‐(2,4‐difluorophenyl)tetrahydrofuran‐3‐yl)methoxy)phenyl)piperazin‐1‐yl)phenyl)‐5‐oxo‐4,5‐dihydro‐1H‐1,2,4‐triazol‐1‐yl)pentan‐2‐yl‐4‐methylbenzenesulfonate, were synthesized and characterized. The genotoxicity which was evaluated by two (quantitative) structure‐activity relationships prediction methodologies showed positive. Furthermore, a novel high‐performance liquid chromatography‐tandem mass spectrometry limit test method for detecting these two impurities in Posaconazole has been established and validated. The chromatographic separation of analytes was conducted on an ACQUITY BEH C18 column, and performed with 0.05% methanoic acid‐water and 0.05% methanoic acid‐acetonitrile as mobile phases A and B, respectively. Six batches of commercial‐scale Posaconazole samples were detected by the validated method and the results were in accordance with the Food and Drug Administration acceptance criteria for the genotoxic impurities in drug substances. Finally, a tentative mechanism for these two impurities was proposed, they are generally accepted to undergo an SN2‐type reaction, resulting in 7‐methylguanine as the predominant adduct in double‐stranded DNA.
磺酸酯类是一类有机杂质，其中包括强效致突变物质，在药物开发过程中通常需要将其控制在较低的ppm水平。在这项研究中，我们发现了泊沙康唑中的两种磺酸酯类基因毒性杂质，例如：((3S,5R)-5-((1H-1,2,4-三唑-1-基)甲基)-5-(2,4-二氟苯基)四氢呋喃-3-基)甲基-4-甲基苯磺酸酯和(2S,3S)-3-(4-(4-(4-(((3R、合成并鉴定了(2S,3S)-3-(4-(4-(((3R, 5R)-5-((1H-1,2,4-三唑-1-基)甲基)-5-(2,4-二氟苯基)四氢呋喃-3-基)甲氧基)苯基)哌嗪-1-基)苯基)-5-氧代-4,5-二氢-1H-1,2,4-三唑-1-基)戊烷-2-基-4-甲基苯磺酸盐。通过两种（定量）结构-活性关系预测方法对其遗传毒性进行了评估，结果呈阳性。此外，还建立并验证了检测泊沙康唑中这两种杂质的新型高效液相色谱-串联质谱限值测试方法。分析物的色谱分离采用 ACQUITY BEH C18 色谱柱，流动相 A 和 B 分别为 0.05% 甲酸-水和 0.05% 甲酸-乙腈。采用该方法检测了6批次商业规模的泊沙康唑样品，结果符合美国食品药品管理局对药物中基因毒性杂质的验收标准。最后，初步提出了这两种杂质的作用机制，一般认为它们会发生 SN2-型反应，导致 7-甲基鸟嘌呤成为双链 DNA 中的主要加合物。
{"title":"Two genotoxic impurities of sulfonate esters in Posaconazole: Synthesis, method validation and mechanism of action","authors":"Fang Li, Weifeng Liu, Kangle Zheng, Hengzhen Luo","doi":"10.1002/sscp.202400040","DOIUrl":"https://doi.org/10.1002/sscp.202400040","url":null,"abstract":"Sulfonate esters are a class of organic impurities that includes highly potent mutagenic substances that typically need to be controlled down to a low ppm level in pharmaceutical development. In this work, two genotoxic impurities of sulfonate esters in Posaconazole, for example, ((3S,5R)‐5‐((1H‐1,2,4‐triazol‐1‐yl)methyl)‐5‐(2,4‐difluorophenyl)tetrahydrofuran‐3‐yl)methyl‐4‐methylbenzenesulfonate and (2S,3S)‐3‐ (4‐(4‐(4‐(4‐(((3R,5R)‐5‐((1H‐1,2,4‐triazol‐1‐yl)methyl)‐5‐(2,4‐difluorophenyl)tetrahydrofuran‐3‐yl)methoxy)phenyl)piperazin‐1‐yl)phenyl)‐5‐oxo‐4,5‐dihydro‐1H‐1,2,4‐triazol‐1‐yl)pentan‐2‐yl‐4‐methylbenzenesulfonate, were synthesized and characterized. The genotoxicity which was evaluated by two (quantitative) structure‐activity relationships prediction methodologies showed positive. Furthermore, a novel high‐performance liquid chromatography‐tandem mass spectrometry limit test method for detecting these two impurities in Posaconazole has been established and validated. The chromatographic separation of analytes was conducted on an ACQUITY BEH C18 column, and performed with 0.05% methanoic acid‐water and 0.05% methanoic acid‐acetonitrile as mobile phases A and B, respectively. Six batches of commercial‐scale Posaconazole samples were detected by the validated method and the results were in accordance with the Food and Drug Administration acceptance criteria for the genotoxic impurities in drug substances. Finally, a tentative mechanism for these two impurities was proposed, they are generally accepted to undergo an SN2‐type reaction, resulting in 7‐methylguanine as the predominant adduct in double‐stranded DNA.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140992051","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A. Sen, Tantul Sarkar, D. Sen, R. Maheshwari, A. Zanwar, Rajesh L. Dumpala
A combination of fixed dose tablet containing 0.5 mg lobeglitazone sulfate (LBZ) and 1 mg glimepiride (GLM) has demonstrated efficacy in enhancing glycemic control in diabetes. The projected work aimed to develop and validate a high‐performance thin‐layer chromatographic (HPTLC) methodology for the precise quantification of both the drugs in tablet formulations. The HPTLC analysis utilized aluminium plates layered with silica gel 60F254, and the solvent system consisted of ethyl acetate, benzene, and hexane (4:3:1 v/v/v) followed by densitometric scanning at 238 nm. The Rf value was found to be 0.68 ± 0.001 for LBZ and 0.48 ± 0.002 for GLM. The methodology exhibited linearity in the range of 100–2000 ng/band for LBZ and 200–4000 ng/band for GLM, with correlation coefficients of 0.9988 and 0.9981, respectively. Exceptional sensitivity was observed, with detection limits of 23.86 ng/band for LBZ and 58.26 ng/band for GLM, along with quantification limits of 72.32 ng/band for LBZ and 176.55 ng/band for GLM. The method demonstrated precision (% relative standard deviation of peak area < 2) and accuracy (recovery between 97% and 102%). The suggested method is suitable for quantifying both the drugs in tablets, making it useful for routine quality control in laboratories.
{"title":"Quantitative determination of lobeglitazone sulfate and glimepiride in combined tablet by robust high‐performance thin layer chromatographic method","authors":"A. Sen, Tantul Sarkar, D. Sen, R. Maheshwari, A. Zanwar, Rajesh L. Dumpala","doi":"10.1002/sscp.202400059","DOIUrl":"https://doi.org/10.1002/sscp.202400059","url":null,"abstract":"A combination of fixed dose tablet containing 0.5 mg lobeglitazone sulfate (LBZ) and 1 mg glimepiride (GLM) has demonstrated efficacy in enhancing glycemic control in diabetes. The projected work aimed to develop and validate a high‐performance thin‐layer chromatographic (HPTLC) methodology for the precise quantification of both the drugs in tablet formulations. The HPTLC analysis utilized aluminium plates layered with silica gel 60F254, and the solvent system consisted of ethyl acetate, benzene, and hexane (4:3:1 v/v/v) followed by densitometric scanning at 238 nm. The Rf value was found to be 0.68 ± 0.001 for LBZ and 0.48 ± 0.002 for GLM. The methodology exhibited linearity in the range of 100–2000 ng/band for LBZ and 200–4000 ng/band for GLM, with correlation coefficients of 0.9988 and 0.9981, respectively. Exceptional sensitivity was observed, with detection limits of 23.86 ng/band for LBZ and 58.26 ng/band for GLM, along with quantification limits of 72.32 ng/band for LBZ and 176.55 ng/band for GLM. The method demonstrated precision (% relative standard deviation of peak area < 2) and accuracy (recovery between 97% and 102%). The suggested method is suitable for quantifying both the drugs in tablets, making it useful for routine quality control in laboratories.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140990557","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The simultaneous determination of Mometasone furoate (MOM) and Olopatadine hydrochloride (OLO) in a combined dose has been developed and validated using a specific, precise, accurate, fast, reliable, and economical high‐performance liquid chromatography technique. Methanol:water:acetonitrile (20:25:55, v/v/v) was used as the mobile phase during the separation. The procedure was performed using a low‐pressure gradient elution on the reversed‐phase Phenomenex C18 column. At 238 nm, separated components were densitometrically measured. The flow rate was fixed at 1.0 mL/min with a continuous run up to 10 min, while the retention time was located near about 3.2 and 6.1 min for OLO and MOM, respectively. The method was validated for Linearity and range, precision, reproducibility, specificity, accuracy, limit of detection, limit of quantification, and robustness as per the International Council for Harmonization Q2(R1) guideline. MOM and OLO regression coefficients (r2) were found to be 0.9994 and 0.9997, over the range of 2.5–15 and 33.25–199.5 µg/mL, respectively. MOM and OLO percentage recoveries were measured to be 99.49 ± 0.14 and 99.98 ± 0.22, respectively. The method can be successfully applied for routine analysis of the quantitative determination of MOM and OLO in a combined dose.
{"title":"Simultaneous estimation of mometasone furoate and olopatadine hydrochloride by reversed‐phase high‐performance liquid chromatography","authors":"Bhoomi Patel, Ruchi Patel","doi":"10.1002/sscp.202300207","DOIUrl":"https://doi.org/10.1002/sscp.202300207","url":null,"abstract":"The simultaneous determination of Mometasone furoate (MOM) and Olopatadine hydrochloride (OLO) in a combined dose has been developed and validated using a specific, precise, accurate, fast, reliable, and economical high‐performance liquid chromatography technique. Methanol:water:acetonitrile (20:25:55, v/v/v) was used as the mobile phase during the separation. The procedure was performed using a low‐pressure gradient elution on the reversed‐phase Phenomenex C18 column. At 238 nm, separated components were densitometrically measured. The flow rate was fixed at 1.0 mL/min with a continuous run up to 10 min, while the retention time was located near about 3.2 and 6.1 min for OLO and MOM, respectively. The method was validated for Linearity and range, precision, reproducibility, specificity, accuracy, limit of detection, limit of quantification, and robustness as per the International Council for Harmonization Q2(R1) guideline. MOM and OLO regression coefficients (r2) were found to be 0.9994 and 0.9997, over the range of 2.5–15 and 33.25–199.5 µg/mL, respectively. MOM and OLO percentage recoveries were measured to be 99.49 ± 0.14 and 99.98 ± 0.22, respectively. The method can be successfully applied for routine analysis of the quantitative determination of MOM and OLO in a combined dose.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140991385","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jemere Kochito, A. Gure, Tamene Tadesse Beyene, O. Femi
Wastewater from the textile and dyeing industries contains hazardous dyes. This study aims to determine the effectiveness of magnetic biochar nanocomposites synthesized from khat leftovers (KLs) and coffee husks (CHs) in removing methylene blue (MB) from wastewater. Magnetic biochar nanocomposites were synthesized by pretreating 25 g of biomass with a 12.5 mmol mixture of FeS and FeCl3 at a 1:1 molar ratio, followed by pyrolyzing at 300°C for 1 h. The resulting products were analyzed using X‐ray diffraction, Fourier transform infrared, scanning electron microscope, and Brunauer‐Emmett‐Teller. The results showed that the adsorbents are amorphous, and the activated biochars, are more porous and contain various functional groups such as C‐O, C = C, O‐H, C‐H, and Fe‐O. When 0.2 g of pristine biochars of CH and KL were applied to 20 mL aqueous solutions containing 20 mg/L of MB at pH 7.5 and 25°C, they removed 44.73% and 75.26% of MB, respectively. However, the resulting nanocomposites exhibited a maximum removal efficiency of 99.10% and 99.23% with magnetic iron oxide‐CH biochar nanocomposite (Fe3O4‐CHBNC) and magnetic iron oxide‐KL biochar nanocomposite (Fe3O4‐KLBNC), respectively, with maximum adsorption capacities of 51.02 and 78.13 mg/g. The reusability study also showed removal efficiencies of 77.57% and 83.49% up to six‐cycle reuse.
{"title":"Magnetic iron‐oxide coffee husk and khat waste biochar nanocomposites for removal of methylene blue from aqueous solution","authors":"Jemere Kochito, A. Gure, Tamene Tadesse Beyene, O. Femi","doi":"10.1002/sscp.202300246","DOIUrl":"https://doi.org/10.1002/sscp.202300246","url":null,"abstract":"Wastewater from the textile and dyeing industries contains hazardous dyes. This study aims to determine the effectiveness of magnetic biochar nanocomposites synthesized from khat leftovers (KLs) and coffee husks (CHs) in removing methylene blue (MB) from wastewater. Magnetic biochar nanocomposites were synthesized by pretreating 25 g of biomass with a 12.5 mmol mixture of FeS and FeCl3 at a 1:1 molar ratio, followed by pyrolyzing at 300°C for 1 h. The resulting products were analyzed using X‐ray diffraction, Fourier transform infrared, scanning electron microscope, and Brunauer‐Emmett‐Teller. The results showed that the adsorbents are amorphous, and the activated biochars, are more porous and contain various functional groups such as C‐O, C = C, O‐H, C‐H, and Fe‐O. When 0.2 g of pristine biochars of CH and KL were applied to 20 mL aqueous solutions containing 20 mg/L of MB at pH 7.5 and 25°C, they removed 44.73% and 75.26% of MB, respectively. However, the resulting nanocomposites exhibited a maximum removal efficiency of 99.10% and 99.23% with magnetic iron oxide‐CH biochar nanocomposite (Fe3O4‐CHBNC) and magnetic iron oxide‐KL biochar nanocomposite (Fe3O4‐KLBNC), respectively, with maximum adsorption capacities of 51.02 and 78.13 mg/g. The reusability study also showed removal efficiencies of 77.57% and 83.49% up to six‐cycle reuse.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140992092","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Shivesh Dessai, V. Mannur, Rahul Koli, Manasi Dhond, Poorvika Badiger
The aim of this study was to develop and validate a robust reversed‐phase high‐performance liquid chromatography (RP‐HPLC) method for the simultaneous estimation of neomycin sulfate (NEO) and beclomethasone dipropionate (BECLO) in both bulk drug and pharmaceutical dosage forms. The analysis was conducted using the Box‐Behnken design. The separation of NEO and BECLO was conducted on a Phenomenex Luna C‐18 column (4.6 × 150 mm, 5 µm), employing a mobile phase comprising a mixture of methanol and trifluoroacetic acid in a ratio of 88:12% v/v. The separation was performed at a flow rate of 0.6 mL/min. NEO and BECLO were analyzed at a wavelength of 240 nm employing a photodiode array detector. The validation of the methodology followed the guidelines outlined in the International Council for Harmonization Q2 R (1). The validation process involved assessing critical parameters such as linearity, accuracy, system suitability, precision, and robustness. The results for each parameter were found to be within the acceptable range. The results indicate that the established RP‐HPLC method can effectively be employed for the routine analysis of NEO and BECLO in bulk drug and pharmaceutical dosage forms.
{"title":"Quality by design‐engineered reversed‐phase high‐performance liquid chromatography method development and validation for simultaneous estimation of neomycin sulfate and beclomethasone dipropionate in bulk and pharmaceutical dosage form","authors":"Shivesh Dessai, V. Mannur, Rahul Koli, Manasi Dhond, Poorvika Badiger","doi":"10.1002/sscp.202400001","DOIUrl":"https://doi.org/10.1002/sscp.202400001","url":null,"abstract":"The aim of this study was to develop and validate a robust reversed‐phase high‐performance liquid chromatography (RP‐HPLC) method for the simultaneous estimation of neomycin sulfate (NEO) and beclomethasone dipropionate (BECLO) in both bulk drug and pharmaceutical dosage forms. The analysis was conducted using the Box‐Behnken design. The separation of NEO and BECLO was conducted on a Phenomenex Luna C‐18 column (4.6 × 150 mm, 5 µm), employing a mobile phase comprising a mixture of methanol and trifluoroacetic acid in a ratio of 88:12% v/v. The separation was performed at a flow rate of 0.6 mL/min. NEO and BECLO were analyzed at a wavelength of 240 nm employing a photodiode array detector. The validation of the methodology followed the guidelines outlined in the International Council for Harmonization Q2 R (1). The validation process involved assessing critical parameters such as linearity, accuracy, system suitability, precision, and robustness. The results for each parameter were found to be within the acceptable range. The results indicate that the established RP‐HPLC method can effectively be employed for the routine analysis of NEO and BECLO in bulk drug and pharmaceutical dosage forms.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140990866","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Codonopsis Radix (CR) is often used as both a medicine and a food ingredient. However, identifying CR can be difficult due to various factors such as variety, sulfur fumigation, and storage time. Consequently, a comprehensive strategy based on fingerprinting and chemometric approaches was developed to distinguish different CRs. First, the fingerprints of CR were acquired by high‐performance liquid chromatography (HPLC). Secondly, various chemical pattern recognition methods were employed to identify CR. Additionally, 14 and 16 major compounds were identified as marker compounds to differentiate between different varieties and sulfur‐fumigated samples, respectively. Furthermore, the amount of Lobetyolin present in different samples was determined, showing that the content of Lobetyolin varied significantly across the samples. Codonopsis pilosula Nannf. var. modesta (Nannf.) L.T.Shen had the highest content of Lobetyolin, followed by Codonopsis tangshen Oliv., and Codonopsis pilosula (Franch.) Nannf. In addition, the content of Lobetyolin was highest when it was non‐sulfur‐fumigated and stored for 0 years. Conclusively, HPLC fingerprint in conjunction with chemical pattern recognition and component content determination, can be employed to differentiate different varieties and sulfur‐fumigated CR. Additionally, it is a reliable, comprehensive, simple, and rapid method for the identification of CR.
{"title":"Identification of Codonopsis Radix from different sources by integrating high‐performance liquid chromatography fingerprinting with chemometric approaches and Lobetyolin determination","authors":"Xuxia Liu, Xiaoling Liu, Xin Wang, Zhengjun Chen, Danhui Nan, Wenrong Luo, Fude Yang","doi":"10.1002/sscp.202400027","DOIUrl":"https://doi.org/10.1002/sscp.202400027","url":null,"abstract":"Codonopsis Radix (CR) is often used as both a medicine and a food ingredient. However, identifying CR can be difficult due to various factors such as variety, sulfur fumigation, and storage time. Consequently, a comprehensive strategy based on fingerprinting and chemometric approaches was developed to distinguish different CRs. First, the fingerprints of CR were acquired by high‐performance liquid chromatography (HPLC). Secondly, various chemical pattern recognition methods were employed to identify CR. Additionally, 14 and 16 major compounds were identified as marker compounds to differentiate between different varieties and sulfur‐fumigated samples, respectively. Furthermore, the amount of Lobetyolin present in different samples was determined, showing that the content of Lobetyolin varied significantly across the samples. Codonopsis pilosula Nannf. var. modesta (Nannf.) L.T.Shen had the highest content of Lobetyolin, followed by Codonopsis tangshen Oliv., and Codonopsis pilosula (Franch.) Nannf. In addition, the content of Lobetyolin was highest when it was non‐sulfur‐fumigated and stored for 0 years. Conclusively, HPLC fingerprint in conjunction with chemical pattern recognition and component content determination, can be employed to differentiate different varieties and sulfur‐fumigated CR. Additionally, it is a reliable, comprehensive, simple, and rapid method for the identification of CR.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140663507","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yu‐Ting Li, Ming‐Xiao Zhang, Ling Su, Sheng‐Yu Zheng, Shengyuan Xiao
Malonyl ginsenosides (mRs) are physiologically active constituents of Asian and American ginseng (P. quinquefolius). They are also important quality markers for the herbs from the Panax genus. Their contents are relevant to several essential quality characteristics of ginseng, for example, the original species, the growing age, the planting areas, the cultivation methods, and the processing conditions. However, when extracted from the herb, an mR is very unstable to lose the malonyl group. This property hampers the structural and quantitative determination of an mR. Herein, We report a trapping and on‐column hydrolysis coupled with a high‐performance liquid chromatography‐tandem mass spectrometry (HPLC‐MS/MS) method. With this method, 19 mRs have been identified from Panax ginseng roots. The isomers of some mRs with identical MS/MS characteristics have been differentiated. The quantities of these mRs have also been determined without references using this method. The quantitative results can be traced to the quantity of certified neutral ginsenoside reference materials. The method has been well‐validated. In addition, unique low‐abundance acetyl ginsenoside Rg1 and malonyl pseudoginsenoside F11 were identified from P. ginseng and P. quinquefolius, respectively.
{"title":"Trapping and on‐column hydrolysis strategy coupled with high‐performance liquid chromatography‐tandem mass spectrometry for new ginsenosides identification and quantification","authors":"Yu‐Ting Li, Ming‐Xiao Zhang, Ling Su, Sheng‐Yu Zheng, Shengyuan Xiao","doi":"10.1002/sscp.202300166","DOIUrl":"https://doi.org/10.1002/sscp.202300166","url":null,"abstract":"Malonyl ginsenosides (mRs) are physiologically active constituents of Asian and American ginseng (P. quinquefolius). They are also important quality markers for the herbs from the Panax genus. Their contents are relevant to several essential quality characteristics of ginseng, for example, the original species, the growing age, the planting areas, the cultivation methods, and the processing conditions. However, when extracted from the herb, an mR is very unstable to lose the malonyl group. This property hampers the structural and quantitative determination of an mR. Herein, We report a trapping and on‐column hydrolysis coupled with a high‐performance liquid chromatography‐tandem mass spectrometry (HPLC‐MS/MS) method. With this method, 19 mRs have been identified from Panax ginseng roots. The isomers of some mRs with identical MS/MS characteristics have been differentiated. The quantities of these mRs have also been determined without references using this method. The quantitative results can be traced to the quantity of certified neutral ginsenoside reference materials. The method has been well‐validated. In addition, unique low‐abundance acetyl ginsenoside Rg1 and malonyl pseudoginsenoside F11 were identified from P. ginseng and P. quinquefolius, respectively.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140432912","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Sulfonate esters, one of the genetic impurities, have gained significant attention in recent years due to their potential to cause genetic mutations and cancer. In this study, we reported a novel on‐line column‐switching liquid chromatography method for the quantitative analysis of three p‐toluene sulfonate alkyl esters in active pharmaceutical ingredients (APIs). The sensitivity was improved by large‐volume injection. A diluting modulation‐based sampling procedure was specifically devised to mitigate the impact of solvent effects and resolve the poor stability of isopropyl p‐toluene sulfonate alkyl ester. The established method was validated in terms of linearity, sensitivity, accuracy, stability, and robustness. The limit of quantitation level was determined to be 1 ng/mL (equivalent to 1 ppm relative to 1 mg/mL API samples). Besides, the method was applied for four APIs Tosuloxacin toluene sulfonate, Lapatinib toluene sulfonate, Nirapalib toluene sulfonate, and Capecitabine. The recoveries of all target analytes in the four‐drug substances were within 89%–110%. The expanded uncertainties of the measurements ranged from 6.8% to 8.4% at a coverage level of k = 2 and a confidence level of approximately 95%. The method described in this paper was compared with other published literature, demonstrating its simplicity and ease of standardization which could be further applied in the quality control and safety assessment of drug substances.
{"title":"Trace determination of genotoxic impurity p‐toluene sulfonate alkyl esters in four active pharmaceutical ingredients by using on‐line column switching liquid chromatography","authors":"Yifei Jiang, Xuejia Zhao, Shengnan Sun, Xiaofang Lian, Huiyi Liu, Ruifang Zheng, Yue Wang, Jing Yao, Guangzhi Shan","doi":"10.1002/sscp.202300245","DOIUrl":"https://doi.org/10.1002/sscp.202300245","url":null,"abstract":"Sulfonate esters, one of the genetic impurities, have gained significant attention in recent years due to their potential to cause genetic mutations and cancer. In this study, we reported a novel on‐line column‐switching liquid chromatography method for the quantitative analysis of three p‐toluene sulfonate alkyl esters in active pharmaceutical ingredients (APIs). The sensitivity was improved by large‐volume injection. A diluting modulation‐based sampling procedure was specifically devised to mitigate the impact of solvent effects and resolve the poor stability of isopropyl p‐toluene sulfonate alkyl ester. The established method was validated in terms of linearity, sensitivity, accuracy, stability, and robustness. The limit of quantitation level was determined to be 1 ng/mL (equivalent to 1 ppm relative to 1 mg/mL API samples). Besides, the method was applied for four APIs Tosuloxacin toluene sulfonate, Lapatinib toluene sulfonate, Nirapalib toluene sulfonate, and Capecitabine. The recoveries of all target analytes in the four‐drug substances were within 89%–110%. The expanded uncertainties of the measurements ranged from 6.8% to 8.4% at a coverage level of k = 2 and a confidence level of approximately 95%. The method described in this paper was compared with other published literature, demonstrating its simplicity and ease of standardization which could be further applied in the quality control and safety assessment of drug substances.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140435216","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hedysari Radix is a commonly used traditional Chinese medicine that improves immunity; formononetin, ononin, calycosin, medicarpin, and vanillic acid play an important role in achieving this effect. Herein, a precise and sensitive ultra‐high‐performance‐tandem mass spectrometry method was developed and validated for the determination of five bioactive components that were extracted from plasma using a protein precipitation method. A Waters CORTES C18 (4.6 × 50 mm, 2.7 µm) and a mobile phase composed of methanol and water (containing 0.2% formic acid) were used for the separation. The method was linear within the concentration range of 19.53–625.00 ng/mL for formononetin; 0.01–3.13 ng/mL for ononin; 0.01–3.13 ng/mL for calycosin; 0.16–5.00 ng/mL for medicarpin; and 19.53–625.00 ng/mL for vanillic acid. This method has a lower limit of quantification, is simple, and has a short analysis time and a high degree of separation. The intra‐day precisions and inter‐day precisions of quality control samples were traced to be below 8.58% and 12.64%, respectively. Fidelity intervened from −8.61% to 10%. Finally, the developed method was used to determine the concentrations of the five bioactive components in rat plasma after the administration of rubbing‐ and non‐rubbing processed Hedysari Radix.
{"title":"Development and validation of a simple ultra‐high‐performance‐tandem mass spectrometry method for the simultaneous determination of five bioactive components in rat plasma of Hedysari Radix","authors":"Xudong Luo, Chengyi Li, Peng Qi, Tingting Liang, Xiaoli Feng, Mingwei Wang, Shubin Liu, Zhengze Qiang, Miaoting Jia, Xiaocheng Wei, Xu Li, Jungang He, Yan Wang","doi":"10.1002/sscp.202300219","DOIUrl":"https://doi.org/10.1002/sscp.202300219","url":null,"abstract":"Hedysari Radix is a commonly used traditional Chinese medicine that improves immunity; formononetin, ononin, calycosin, medicarpin, and vanillic acid play an important role in achieving this effect. Herein, a precise and sensitive ultra‐high‐performance‐tandem mass spectrometry method was developed and validated for the determination of five bioactive components that were extracted from plasma using a protein precipitation method. A Waters CORTES C18 (4.6 × 50 mm, 2.7 µm) and a mobile phase composed of methanol and water (containing 0.2% formic acid) were used for the separation. The method was linear within the concentration range of 19.53–625.00 ng/mL for formononetin; 0.01–3.13 ng/mL for ononin; 0.01–3.13 ng/mL for calycosin; 0.16–5.00 ng/mL for medicarpin; and 19.53–625.00 ng/mL for vanillic acid. This method has a lower limit of quantification, is simple, and has a short analysis time and a high degree of separation. The intra‐day precisions and inter‐day precisions of quality control samples were traced to be below 8.58% and 12.64%, respectively. Fidelity intervened from −8.61% to 10%. Finally, the developed method was used to determine the concentrations of the five bioactive components in rat plasma after the administration of rubbing‐ and non‐rubbing processed Hedysari Radix.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140438634","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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