Abstract This study was designed to enable the development of a simple, fast, and environmentally friendly analytical technique utilizing dispersive liquid‐liquid microextraction based on surface floating organic droplets for selective and quantitative enrichment of trace level pesticide contaminants from different fruit juice samples for subsequent detection by high performance liquid chromatography, combined with a diode array detector. The selective extraction was necessitated in order to isolate the seven multiclass pesticide residues frequently occurring in fruit juice samples. The effects of experimental parameters such as pH of sample solution, type and volume of extraction and dispersive solvents, ionic strength and extraction time were optimized. The optimized method was validated using spiked blank sample and satisfactory results for accuracy, with recoveries ranging from 87.23% to 99.45%, with %relative standard deviation between 1.37 and 8.39, precision in terms of %relative standard deviation ≤ 10.78 and linearity at concentration levels from 3 to 1500 ng/ml, which corresponded with correlation coefficients ≥ 0.998. The limits of detection and the limits of quantification were ranged from 1.3×10 −2 to 5.3×10 −2 and 4.2×10 −2 to 1.8×10 −1 μg/L, respectively. At the end, the method was successfully applied to analyze real fruit juice samples and target analytes were not detected in real samples.
{"title":"Fast surface floating organic droplets based dispersive liquid‐liquid microextraction for trace enrichment of multiclass pesticide residues from different fruit juice samples followed by high performance liquid chromatography–diode array detection analysis","authors":"Habtamu Bekele, Negussie Megersa","doi":"10.1002/sscp.202300042","DOIUrl":"https://doi.org/10.1002/sscp.202300042","url":null,"abstract":"Abstract This study was designed to enable the development of a simple, fast, and environmentally friendly analytical technique utilizing dispersive liquid‐liquid microextraction based on surface floating organic droplets for selective and quantitative enrichment of trace level pesticide contaminants from different fruit juice samples for subsequent detection by high performance liquid chromatography, combined with a diode array detector. The selective extraction was necessitated in order to isolate the seven multiclass pesticide residues frequently occurring in fruit juice samples. The effects of experimental parameters such as pH of sample solution, type and volume of extraction and dispersive solvents, ionic strength and extraction time were optimized. The optimized method was validated using spiked blank sample and satisfactory results for accuracy, with recoveries ranging from 87.23% to 99.45%, with %relative standard deviation between 1.37 and 8.39, precision in terms of %relative standard deviation ≤ 10.78 and linearity at concentration levels from 3 to 1500 ng/ml, which corresponded with correlation coefficients ≥ 0.998. The limits of detection and the limits of quantification were ranged from 1.3×10 −2 to 5.3×10 −2 and 4.2×10 −2 to 1.8×10 −1 μg/L, respectively. At the end, the method was successfully applied to analyze real fruit juice samples and target analytes were not detected in real samples.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135363418","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}
{"title":"Development and validation of a liquid chromatography–tandem mass spectrometry method of a panel of commonly prescribed benzodiazepines in urine samples","authors":"C. Karakukcu, H. Saraçoglu","doi":"10.1002/sscp.202300036","DOIUrl":"https://doi.org/10.1002/sscp.202300036","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":" ","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48330228","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}
{"title":"LC method for the quantification of Quercetin, Berberine, and Phytosterol in lyophilized liposome","authors":"Puja Bhavsar, L. Jha, Lima Patel, F. Tandel","doi":"10.1002/sscp.202300047","DOIUrl":"https://doi.org/10.1002/sscp.202300047","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":" ","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42363202","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}
Abstract Isosorbide dinitrate and hydralazine hydrochloride tablets are approved for the treatment of heart failure, prolonged hospitalization for heart failure, and enhanced patient‐reported functional status. It has been administered orally. Isosorbide dinitrate and hydralazine hydrochloride tablets contained two additional major unknown peaks (Degradation Product 1 and Degradation Product 2) in the stability studies (25°C/60% relative humidity and 40°C/75% relative humidity). These two unknown degradation peaks formed due to the heat (thermal) and humidity stress of hydralazine hydrochloride. Liquid chromatography separated these unknown degradant peaks. Initially, liquid chromatography‐mass spectrometry assessed the degradation pathways and mass of two degradants. Afterward, preparative‐liquid chromatography isolated the two major unknown degradation impurities formed under heat (thermal) and humidity stress conditions. Further, to confirm the structures, nuclear magnetic resonance spectroscopy evaluated these two degradants. The liquid chromatography‐mass spectrometry and nuclear magnetic resonance spectral data confirmed that the two degradation impurities are hydralazine lactosone ring‐opened adduct (Degradation Product 1) and s‐triazolo [3,4‐α] phthalazine (Degradation Product 2).
{"title":"Identification and structural characterization of lactose adduct impurities in isosorbide dinitrate and hydralazine hydrochloride tablets by liquid chromatography‐mass spectrometry and nuclear magnetic resonance studies","authors":"Venkatarao Muppavarapu, Gangu Naidu Challa, Mukteeshwar Gande, Praveen Reddy Billa, Venkatesh Madhavacharya Joshi, Thirupathi Ch, Swamy Ponnapalli Veerabhadra, Srinivasa Rao Y","doi":"10.1002/sscp.202200144","DOIUrl":"https://doi.org/10.1002/sscp.202200144","url":null,"abstract":"Abstract Isosorbide dinitrate and hydralazine hydrochloride tablets are approved for the treatment of heart failure, prolonged hospitalization for heart failure, and enhanced patient‐reported functional status. It has been administered orally. Isosorbide dinitrate and hydralazine hydrochloride tablets contained two additional major unknown peaks (Degradation Product 1 and Degradation Product 2) in the stability studies (25°C/60% relative humidity and 40°C/75% relative humidity). These two unknown degradation peaks formed due to the heat (thermal) and humidity stress of hydralazine hydrochloride. Liquid chromatography separated these unknown degradant peaks. Initially, liquid chromatography‐mass spectrometry assessed the degradation pathways and mass of two degradants. Afterward, preparative‐liquid chromatography isolated the two major unknown degradation impurities formed under heat (thermal) and humidity stress conditions. Further, to confirm the structures, nuclear magnetic resonance spectroscopy evaluated these two degradants. The liquid chromatography‐mass spectrometry and nuclear magnetic resonance spectral data confirmed that the two degradation impurities are hydralazine lactosone ring‐opened adduct (Degradation Product 1) and s‐triazolo [3,4‐α] phthalazine (Degradation Product 2).","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"68 1 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135449274","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}
Abstract Polyvinylpyrrolidone (PVP) is known as a polymer with special adsorption properties for polyphenolic compounds. In this paper, chemical‐bonded stationary phase (PVP@Silica) was prepared and applied to the separation of flavonoids. System constants determined by linear solvation energy relationships with methanol–water mixtures as the mobile show that the column can provide stronger hydrogen bonding and π–π interaction than C18 column. Under reversed‐phase conditions, traditional flavonoids have much longer retention on PVP@Silica than on C18 column with methanol–water mobile phase due to multimodal retention mechanism, including hydrogen bonding and π–π interaction. In addition, a U‐shaped retention curve was observed in acetonitrile–water mobile phase because of the enhanced hydrogen bonding under the high proportion of acetonitrile. The selectivity to polyhydroxy structure gives the stationary phase unique separation ability for flavonoids. The separation orthogonality was further investigated by a sample set containing 33 flavonoids with different substitution structures. The (RP‐PVP@Silica)‐(RP‐C18) system exhibited 60% orthogonality metric (OM) for these flavonoids with methanol–water mobile phase. A high OM of 63.5% was achieved in (RP‐PVP@Silica)‐(HILIC‐PVP@Silica) system. Finally, PVP@Silica was applied to the purification of total flavonoids in Ginkgo biloba extract (GBE). The offline (RP‐PVP@Silica)‐(RP‐C18) two‐dimensional separation system was used for the analysis of flavonoids in GBE.
{"title":"Preparation of polyvinyl pyrrolidone stationary phase and its application in separation and analysis of flavonoids","authors":"Xin Chen, Juntao Li, Mengting Gu, Yiyuan Miao, Yanxiong Ke, Xiangwei Zheng, Jian Xu","doi":"10.1002/sscp.202300059","DOIUrl":"https://doi.org/10.1002/sscp.202300059","url":null,"abstract":"Abstract Polyvinylpyrrolidone (PVP) is known as a polymer with special adsorption properties for polyphenolic compounds. In this paper, chemical‐bonded stationary phase (PVP@Silica) was prepared and applied to the separation of flavonoids. System constants determined by linear solvation energy relationships with methanol–water mixtures as the mobile show that the column can provide stronger hydrogen bonding and π–π interaction than C18 column. Under reversed‐phase conditions, traditional flavonoids have much longer retention on PVP@Silica than on C18 column with methanol–water mobile phase due to multimodal retention mechanism, including hydrogen bonding and π–π interaction. In addition, a U‐shaped retention curve was observed in acetonitrile–water mobile phase because of the enhanced hydrogen bonding under the high proportion of acetonitrile. The selectivity to polyhydroxy structure gives the stationary phase unique separation ability for flavonoids. The separation orthogonality was further investigated by a sample set containing 33 flavonoids with different substitution structures. The (RP‐PVP@Silica)‐(RP‐C18) system exhibited 60% orthogonality metric (OM) for these flavonoids with methanol–water mobile phase. A high OM of 63.5% was achieved in (RP‐PVP@Silica)‐(HILIC‐PVP@Silica) system. Finally, PVP@Silica was applied to the purification of total flavonoids in Ginkgo biloba extract (GBE). The offline (RP‐PVP@Silica)‐(RP‐C18) two‐dimensional separation system was used for the analysis of flavonoids in GBE.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"2 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135449582","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}
{"title":"Miniaturized liquid extraction cartridge with a functional porous polytetrafluoroethylene membrane for the determination of formaldehyde in gaseous samples","authors":"I. Ueta, Shunsuke Kawamura, Yoshihiro Saito","doi":"10.1002/sscp.202300033","DOIUrl":"https://doi.org/10.1002/sscp.202300033","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":" ","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44874861","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}
Qingzhu Hao, Shuo‐Wen Wang, Li-Qing Yu, Xiao‐Qin Yang, Y. Lv
{"title":"Immobilization of zeolitic imidazolate framework‐90 onto modified stainless steel wire via covalent bonding for solid‐phase microextraction of biomarkers in exhalation of lung cancer patients","authors":"Qingzhu Hao, Shuo‐Wen Wang, Li-Qing Yu, Xiao‐Qin Yang, Y. Lv","doi":"10.1002/sscp.202300026","DOIUrl":"https://doi.org/10.1002/sscp.202300026","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":" ","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42118921","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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