Pub Date : 2022-01-01DOI: 10.52568/001127/jcsp/44.05.2022
Abdus Salam Abdus Salam
Dimethyl dibenzylidene sorbitol (DMDBS) is one of the most commonly used nucleating agent in polypropylene formulations. In present study, a simple and robust reversed phase liquid chromatography (RP-LC) based analytical method was developed for the quantitative low-level determination of DMDBS. The best separation was achieved on a RP-HPLC column TSK gel G2000 SW, 7.5mm x 30cm, Particle Size 10 and#181;m from TOSOH Bioscience. A 0.05 M NH4AC (pH = 6.6) + 10% ACN solution was used as mobile phase at a flow rate of 1.2 ml/min. UV detection was performed at 216 nm. Retention time was found to be 13.056 min. for DMDBS. The response was a linear function of concentration over the range of 2.00 to 8.00 and#181;g/ml with correlation coefficient of 0.9996 for DMDBS. The LOD and LOQ for DMDBS were found to be 1.00 and#181;g/mL and 2.00 and#181;g/mL respectively. The method is simple, rapid and robust, which is suitable for application in quality control and can also be used for the estimation of DMDBS as a leachable/ extractable from polypropylene (PP) resin and resin products like medical device containers.
二甲基二苄基山梨醇(DMDBS)是聚丙烯配方中最常用的成核剂之一。本研究建立了一种简单、可靠的反相液相色谱(RP-LC)分析方法，用于DMDBS的低浓度定量测定。采用反相高效液相色谱柱TSK gel G2000 SW, 7.5mm x 30cm，粒径10和#181;m，来自TOSOH Bioscience。以0.05 M NH4AC (pH = 6.6) + 10% ACN溶液为流动相，流速为1.2 ml/min。在216 nm处进行紫外检测。DMDBS的滞留时间为13.056 min。DMDBS浓度在2.00 ~ 8.00和181 g/ml范围内呈线性关系，相关系数为0.9996。DMDBS的LOD和LOQ分别为1.00和#181 g/mL和2.00和#181 g/mL。该方法简便、快速、鲁棒性好，适用于质量控制，也可用于聚丙烯(PP)树脂和医疗器械容器等树脂制品中可浸出/可萃取的DMDBS的估计。
{"title":"Reversed Phase-HPLC Method for Low Level Quantitation of Dimethyl dibenzylidene Sorbitol","authors":"Abdus Salam Abdus Salam","doi":"10.52568/001127/jcsp/44.05.2022","DOIUrl":"https://doi.org/10.52568/001127/jcsp/44.05.2022","url":null,"abstract":"Dimethyl dibenzylidene sorbitol (DMDBS) is one of the most commonly used nucleating agent in polypropylene formulations. In present study, a simple and robust reversed phase liquid chromatography (RP-LC) based analytical method was developed for the quantitative low-level determination of DMDBS. The best separation was achieved on a RP-HPLC column TSK gel G2000 SW, 7.5mm x 30cm, Particle Size 10 and#181;m from TOSOH Bioscience. A 0.05 M NH4AC (pH = 6.6) + 10% ACN solution was used as mobile phase at a flow rate of 1.2 ml/min. UV detection was performed at 216 nm. Retention time was found to be 13.056 min. for DMDBS. The response was a linear function of concentration over the range of 2.00 to 8.00 and#181;g/ml with correlation coefficient of 0.9996 for DMDBS. The LOD and LOQ for DMDBS were found to be 1.00 and#181;g/mL and 2.00 and#181;g/mL respectively. The method is simple, rapid and robust, which is suitable for application in quality control and can also be used for the estimation of DMDBS as a leachable/ extractable from polypropylene (PP) resin and resin products like medical device containers.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70707817","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001184/jcsp/44.06.2022
Ahmed N Alhakimi Ahmed N Alhakimi, Thikra A Almuhanna Jawza Sh Alnawmasi Thikra A Almuhanna Jawza Sh Alnawmasi, S. E. S. S. A. E. H. L. A. S El Sayed Saeed and Ebtesam H L Alhamzi
A new series complexes of Ni(II), Mn(II), Co(III), Cu(II), Cr(II), Zn(II), Zr(IV), Cd(II), and La(III) prepared by the reaction of the metal salt with a new Schiff base ligand. This Schiff base obtained by the condensation of p-phenylenediamine, 4-chlorobenzaldehyde, and acetyl acetone. The confirmation of the ligand and its metal complexes were characterized by multiple techniques such as, elemental analyses, magnetic susceptibility studies, FTIR 1H, 13C-NMR, XRD, molar conductance, UV-vis spectral analyses, and thermal analyses. The conductivity measurements of the complexes in DMF solutions indicated that the prepared complexes are nonelectrolytes. From the spectral data, an octahedral geometry was suggested for all complexes. The metal complex [(L)2Zr(Cl)2].3H2O showed the highest antifungal activity. The complexes [(L)(HL)Co(Cl)2].3H2O, and [(L)2Cd(H2O)2] showed antibacterial activities higher than the other complexes. All complexes are exhibited potent fungicides and bactericides than the ligand. Complex [(L)2Cd(H2O)2] exhibited considerable cytotoxicity against PC-3, SKOV3, and HeLa cells. The ligand C18H17N2OCl (HL) showed strong toxicity towards PC-3, HeLa cells, and moderate toxicity against SKOV3 cells.
{"title":"Synthesis, Spectroscopic Characterization, and Anticancer Activity of Metal Complexes with a Novel Schiff Base Ligand from -Diketone Derivatives","authors":"Ahmed N Alhakimi Ahmed N Alhakimi, Thikra A Almuhanna Jawza Sh Alnawmasi Thikra A Almuhanna Jawza Sh Alnawmasi, S. E. S. S. A. E. H. L. A. S El Sayed Saeed and Ebtesam H L Alhamzi","doi":"10.52568/001184/jcsp/44.06.2022","DOIUrl":"https://doi.org/10.52568/001184/jcsp/44.06.2022","url":null,"abstract":"A new series complexes of Ni(II), Mn(II), Co(III), Cu(II), Cr(II), Zn(II), Zr(IV), Cd(II), and La(III) prepared by the reaction of the metal salt with a new Schiff base ligand. This Schiff base obtained by the condensation of p-phenylenediamine, 4-chlorobenzaldehyde, and acetyl acetone. The confirmation of the ligand and its metal complexes were characterized by multiple techniques such as, elemental analyses, magnetic susceptibility studies, FTIR 1H, 13C-NMR, XRD, molar conductance, UV-vis spectral analyses, and thermal analyses. The conductivity measurements of the complexes in DMF solutions indicated that the prepared complexes are nonelectrolytes. From the spectral data, an octahedral geometry was suggested for all complexes. The metal complex [(L)2Zr(Cl)2].3H2O showed the highest antifungal activity. The complexes [(L)(HL)Co(Cl)2].3H2O, and [(L)2Cd(H2O)2] showed antibacterial activities higher than the other complexes. All complexes are exhibited potent fungicides and bactericides than the ligand. Complex [(L)2Cd(H2O)2] exhibited considerable cytotoxicity against PC-3, SKOV3, and HeLa cells. The ligand C18H17N2OCl (HL) showed strong toxicity towards PC-3, HeLa cells, and moderate toxicity against SKOV3 cells.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70707890","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001186/jcsp/44.06.2022
Sitara Anjum Sitara Anjum, Sana Ashraf Sana Ashraf, Sajid Rashid Ahmad Sajid Rashid Ahmad, Muhammad Salman and Zahra Majid Muhammad Salman and Zahra Majid
This study was conducted to analyze the efficacy of Polyalthia longifolia branches as an effective biosorbent for elimination of textile dye stuff brilliant yellow. Different operating conditions were tested (adsorbent dose, dye concentration, contact time, pH and temperature) to investigate their relationship with adsorption strength of Polyalthia longifolia and subsequently to eliminate toxic color. The absorbent was also characterized by Fourier Transform Infrared (FTIR). Optimum adsorption was observed at pH 6. Model of kinetic explored the adsorption data showing pseudo 2nd order with high correlation coefficient R2 of 0.996. Langmuir model followed well to equilibrium data relative to Freundlich and Temkin models. Thermodynamic property was also observed, where Gibbs free energy, entropy and enthalpy were analyzed. Through Gibbs free energy it was found that absorbent has endothermic nature. Thermodynamic properties have depicted that adsorption process was natural, endothermic and suitable for treatment of toxic dye.
{"title":"Potential of Polyalthia longifolia Branches as a Biosorbent to Remove Textile Brilliant Yellow Dye from Aqueous Media","authors":"Sitara Anjum Sitara Anjum, Sana Ashraf Sana Ashraf, Sajid Rashid Ahmad Sajid Rashid Ahmad, Muhammad Salman and Zahra Majid Muhammad Salman and Zahra Majid","doi":"10.52568/001186/jcsp/44.06.2022","DOIUrl":"https://doi.org/10.52568/001186/jcsp/44.06.2022","url":null,"abstract":"This study was conducted to analyze the efficacy of Polyalthia longifolia branches as an effective biosorbent for elimination of textile dye stuff brilliant yellow. Different operating conditions were tested (adsorbent dose, dye concentration, contact time, pH and temperature) to investigate their relationship with adsorption strength of Polyalthia longifolia and subsequently to eliminate toxic color. The absorbent was also characterized by Fourier Transform Infrared (FTIR). Optimum adsorption was observed at pH 6. Model of kinetic explored the adsorption data showing pseudo 2nd order with high correlation coefficient R2 of 0.996. Langmuir model followed well to equilibrium data relative to Freundlich and Temkin models. Thermodynamic property was also observed, where Gibbs free energy, entropy and enthalpy were analyzed. Through Gibbs free energy it was found that absorbent has endothermic nature. Thermodynamic properties have depicted that adsorption process was natural, endothermic and suitable for treatment of toxic dye.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70708057","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/000978/jcsp/44.01.2022
Yaoqiang Hu Yaoqiang Hu, Min Guo Min Guo, Xiushen Ye Xiushen Ye, Quan Li Quan Li, Haining Liu Haining Liu, Zhijian Wu Zhijian Wu
Electrosorption can be used for both desalination of seawater and high value element ions enrichment, which has attracted more and more attentions because of its merits of low energy consumption, no pollution and inexpensive. The research focuses on the preparation of novel electrodes and selective electrosorption properties. In this paper, biomass carbon aerogel was prepared by hydrothermal-freeze drying- carbonization method using pomelo peel as raw material. A composite electrosorption electrode was obtained using pomelo peel-based carbon aerogel (PCA) as main component. The surface morphology, crystal structure, specific surface area and functional groups were characterized by Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), Brunauer Emmett Teller (BET) and Fourier Transform Infrared Spectroscopy (FTIR). Then the effects of coexisted alkali/alkaline earth metal ions on the adsorption of Rb+ and Cs+ were studied. The pomelo peel-based carbon aerogel-manganese dioxide (PCA-MnO2) composite electrode shows good adsorption performance on Rb+ and Cs+. When alkali and alkaline earth metal ions coexist, PCA-MnO2 composite electrode exhibits the highest adsorption selectivity of Mg2+. The research content in this work broadens the source of electrosorption electrode and provides a reference for the study of competitive adsorption of alkali/alkaline earth metal ions.
{"title":"Preparation of Pomelo Peel-Based Biomass Carbon Aerogel-MnO2 Composite Electrode and its Adsorption Performance of Rb+ and Cs+","authors":"Yaoqiang Hu Yaoqiang Hu, Min Guo Min Guo, Xiushen Ye Xiushen Ye, Quan Li Quan Li, Haining Liu Haining Liu, Zhijian Wu Zhijian Wu","doi":"10.52568/000978/jcsp/44.01.2022","DOIUrl":"https://doi.org/10.52568/000978/jcsp/44.01.2022","url":null,"abstract":"Electrosorption can be used for both desalination of seawater and high value element ions enrichment, which has attracted more and more attentions because of its merits of low energy consumption, no pollution and inexpensive. The research focuses on the preparation of novel electrodes and selective electrosorption properties. In this paper, biomass carbon aerogel was prepared by hydrothermal-freeze drying- carbonization method using pomelo peel as raw material. A composite electrosorption electrode was obtained using pomelo peel-based carbon aerogel (PCA) as main component. The surface morphology, crystal structure, specific surface area and functional groups were characterized by Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), Brunauer Emmett Teller (BET) and Fourier Transform Infrared Spectroscopy (FTIR). Then the effects of coexisted alkali/alkaline earth metal ions on the adsorption of Rb+ and Cs+ were studied. The pomelo peel-based carbon aerogel-manganese dioxide (PCA-MnO2) composite electrode shows good adsorption performance on Rb+ and Cs+. When alkali and alkaline earth metal ions coexist, PCA-MnO2 composite electrode exhibits the highest adsorption selectivity of Mg2+. The research content in this work broadens the source of electrosorption electrode and provides a reference for the study of competitive adsorption of alkali/alkaline earth metal ions.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70706254","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001070/jcsp/44.04.2022
Ali Mohammed Mahir Fahad Ali Mohammed Mahir Fahad, Ashraf Saad Rasheed and Hameed Hussien Ali Ashraf Saad Rasheed and Hameed Hussien Ali
A rapid method for simultaneous determination of two statin drugs based on zwitterionic chromatography (ZIC) had been developed and validated. The development method included examining the effects of chromatographic conditions, including the percentage of organic modifier, pH values, ionic strength of the acetate buffer, and the predominant retention mechanismand#39;s experimental determination. Separation developed by two zwitterionic stationary phases (100 mm and#215; 4.6 mm I.D., 3.5and#181;). The influence of various spacer lengths was being used as an examination tool on atorvastatin and rosuvastatin retention behaviours. Two zwitterionic stationary phases and a mobile phase consisting of acetonitrile and acetate (pH = 4.75, 40 mM) in a ratio of 80:20 V/V were used to achieve optimum chromatographic conditions. The methods had been validated for linearity, accuracy, and precision. This validation shows that the ZIC-HILIC methods proposed were sufficient for quantification analysis of atorvastatin and rosuvastatin. Quantifications were achieved with U.V. detection at 240 nm over the concentration range of 0.1–7.0 μg mL-1 for atorvastatin and rosuvastatin, respectively.
{"title":"Hydrophilic Interaction Chromatography with Sulfobetaine Zwitterionic Polymer-Bonded Stationary Phases","authors":"Ali Mohammed Mahir Fahad Ali Mohammed Mahir Fahad, Ashraf Saad Rasheed and Hameed Hussien Ali Ashraf Saad Rasheed and Hameed Hussien Ali","doi":"10.52568/001070/jcsp/44.04.2022","DOIUrl":"https://doi.org/10.52568/001070/jcsp/44.04.2022","url":null,"abstract":"A rapid method for simultaneous determination of two statin drugs based on zwitterionic chromatography (ZIC) had been developed and validated. The development method included examining the effects of chromatographic conditions, including the percentage of organic modifier, pH values, ionic strength of the acetate buffer, and the predominant retention mechanismand#39;s experimental determination. Separation developed by two zwitterionic stationary phases (100 mm and#215; 4.6 mm I.D., 3.5and#181;). The influence of various spacer lengths was being used as an examination tool on atorvastatin and rosuvastatin retention behaviours. Two zwitterionic stationary phases and a mobile phase consisting of acetonitrile and acetate (pH = 4.75, 40 mM) in a ratio of 80:20 V/V were used to achieve optimum chromatographic conditions. The methods had been validated for linearity, accuracy, and precision. This validation shows that the ZIC-HILIC methods proposed were sufficient for quantification analysis of atorvastatin and rosuvastatin. Quantifications were achieved with U.V. detection at 240 nm over the concentration range of 0.1–7.0 μg mL-1 for atorvastatin and rosuvastatin, respectively.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70706629","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001004/jcsp/44.02.2022
Cherifa Mahieddine Cherifa Mahieddine, Said Zerkout Said Zerkout, Sidali Rayane Sidali Rayane, Houssam Boulebd Houssam Boulebd, Affaf Laassami Affaf Laassami, Salah Akkal Salah Akkal
The benefits of dinitrones (N,Nand#39;-Diphenyl-2,5-thenylenedinitrone, N,Nand#39;-Dimethyl-1,4-phenylenedinitrone and N,Nand#39;-Dibenzyl-1,4-phenylenedinitrone) in the synthesis were chosen as simple process for synthesis of the purified dihydroxamic acid compounds in a shorter time with a good yield and high purity without need to purification. The most stable conformers of the synthesized compounds and their electronic properties have been determined using DFT/B3LYP calculations. Antimicrobial activity assessment of dihydroxamic acids showed their good efficiency.
{"title":"Synthesis of Dihydroxamic Acids from Dinitrones, Structural Characterization and Antimicrobial Activities","authors":"Cherifa Mahieddine Cherifa Mahieddine, Said Zerkout Said Zerkout, Sidali Rayane Sidali Rayane, Houssam Boulebd Houssam Boulebd, Affaf Laassami Affaf Laassami, Salah Akkal Salah Akkal","doi":"10.52568/001004/jcsp/44.02.2022","DOIUrl":"https://doi.org/10.52568/001004/jcsp/44.02.2022","url":null,"abstract":"The benefits of dinitrones (N,Nand#39;-Diphenyl-2,5-thenylenedinitrone, N,Nand#39;-Dimethyl-1,4-phenylenedinitrone and N,Nand#39;-Dibenzyl-1,4-phenylenedinitrone) in the synthesis were chosen as simple process for synthesis of the purified dihydroxamic acid compounds in a shorter time with a good yield and high purity without need to purification. The most stable conformers of the synthesized compounds and their electronic properties have been determined using DFT/B3LYP calculations. Antimicrobial activity assessment of dihydroxamic acids showed their good efficiency.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70706966","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001123/jcsp/44.05.2022
Shumaila Naz Shumaila Naz, Muhammad Nadir Muhammad Nadir, Pirzada Jamal Ahmed Siddiqui Pirzada Jamal Ahmed Siddiqui, Amir Ahmed Amir Ahmed, Muhammad Noman Syed Muhammad Noman Syed, Munawwer Rasheed Munawwer Rasheed
The blue whale, Balaenoptera musculus (Linnaeus, 1758), is the biggest animal recognized to exist today throughout world’s oceans. High commercial value of lipids has made this species vulnerable. Blubber, a crucial adaptation for mammals living in water, serves as energy reservoir. Surplus energy is deposited in the form of fatty acids (FA) and therefore have been analysed. The compositional analysis also helps in understanding the dietary and structural role of FAs in blubber. Lipid analysis of blubber from stranded, dead blue whale through Thin layer chromatography (TLC) has resulted in identifying 6 constituents. These constituents are a triacyl glyceride (TAG), 2 steroids, and 3 FAs. Approximate analysis of waxy constituents has also been attempted exploiting TLC. Gas chromatography-mass spectrometry (GC-MS) analyses has resulted in identification of 86 compounds, which were further confirmed through the Retention Indices. Altogether 17 SFAs including 4 Branched FAs, 5 MUFAs, and a PUFA were identified. These accounted to a total concentration of 85.7, 86.1, 84.8, and 89.7 % in jaw, abdomen, peduncle, and fluke, respectively. The main reasons for the low quantitative and qualitative content of PUFAs were susceptibility of PUFAs towards oxidation. Thus 8 FAlds, 4 FAlcs, and 3 other oxygenated FAs, which made a total of 2.7, 0.9, 1.3, and 5.2% in jaw, abdomen, peduncle, and fluke, respectively were justified. Further the chromatographic region where PUFAs are expected to resolve has been found masked with significant concentration of anthropogenic compounds, which accounted to 43.4, 35.6, 34.6, and 30.7% in jaw, abdomen, peduncle, and fluke, respectively. These pollutants included 25 hydrocarbons, 4 phthalates, 2 siloxanes, 2 bisphenols, and diphenyl carbonate. 4 natural Prenols were also identified. Altogether 16 constituents with concentration of 14.2, 8.0, 15.7, and 10.8% in jaw, abdomen, peduncle, and fluke, respectively, were remained unidentified. Few constituents were justified through food chain.
{"title":"Lipophilic Constituents of the Blubber from Blue Whale, Balaenoptera musculus, Washed Ashore at Pakistan Coast","authors":"Shumaila Naz Shumaila Naz, Muhammad Nadir Muhammad Nadir, Pirzada Jamal Ahmed Siddiqui Pirzada Jamal Ahmed Siddiqui, Amir Ahmed Amir Ahmed, Muhammad Noman Syed Muhammad Noman Syed, Munawwer Rasheed Munawwer Rasheed","doi":"10.52568/001123/jcsp/44.05.2022","DOIUrl":"https://doi.org/10.52568/001123/jcsp/44.05.2022","url":null,"abstract":"The blue whale, Balaenoptera musculus (Linnaeus, 1758), is the biggest animal recognized to exist today throughout world’s oceans. High commercial value of lipids has made this species vulnerable. Blubber, a crucial adaptation for mammals living in water, serves as energy reservoir. Surplus energy is deposited in the form of fatty acids (FA) and therefore have been analysed. The compositional analysis also helps in understanding the dietary and structural role of FAs in blubber. Lipid analysis of blubber from stranded, dead blue whale through Thin layer chromatography (TLC) has resulted in identifying 6 constituents. These constituents are a triacyl glyceride (TAG), 2 steroids, and 3 FAs. Approximate analysis of waxy constituents has also been attempted exploiting TLC. Gas chromatography-mass spectrometry (GC-MS) analyses has resulted in identification of 86 compounds, which were further confirmed through the Retention Indices. Altogether 17 SFAs including 4 Branched FAs, 5 MUFAs, and a PUFA were identified. These accounted to a total concentration of 85.7, 86.1, 84.8, and 89.7 % in jaw, abdomen, peduncle, and fluke, respectively. The main reasons for the low quantitative and qualitative content of PUFAs were susceptibility of PUFAs towards oxidation. Thus 8 FAlds, 4 FAlcs, and 3 other oxygenated FAs, which made a total of 2.7, 0.9, 1.3, and 5.2% in jaw, abdomen, peduncle, and fluke, respectively were justified. Further the chromatographic region where PUFAs are expected to resolve has been found masked with significant concentration of anthropogenic compounds, which accounted to 43.4, 35.6, 34.6, and 30.7% in jaw, abdomen, peduncle, and fluke, respectively. These pollutants included 25 hydrocarbons, 4 phthalates, 2 siloxanes, 2 bisphenols, and diphenyl carbonate. 4 natural Prenols were also identified. Altogether 16 constituents with concentration of 14.2, 8.0, 15.7, and 10.8% in jaw, abdomen, peduncle, and fluke, respectively, were remained unidentified. Few constituents were justified through food chain.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70707461","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001189/jcsp/44.06.2022
Jing Huang Jing Huang, Jincan Lei Jincan Lei, Shixian Zhao and Yan Li Shixian Zhao and Yan Li
In this paper, a fast detection method for pesticide residues was proposed, and the qualitative and quantitative detection of the pesticide could be got at once by the method of solution of multiple linear regression equations which were obtained by dual wavelength absorbance and fluorescence spectrometry with least squares method. Moreover, it could detect two kinds of mixed pesticides. Four selected pesticides, aldicarb, fenitrothion, fenvalerate, and chlorothalonil were detected by the method. The results shown that there were good linear relationship in the range of 0.01-1 ppm, and R2 ＞ 0.90. And the method could 100% discriminate the four pesticide residues, the limit of detection was below 8 ppb both single one and mixed one. The recoveries of the pesticides in cabbage samples were observed 92.12%-107.50%. And the recoveries of the mixed pesticides in mineral water samples were observed 86.44%-114.10%. The preliminary study demonstrates that the proposed method has excellent potential application for the safety inspection of food.
{"title":"A Fast Detection Method for Pesticide Residues by Spectrometry Technique","authors":"Jing Huang Jing Huang, Jincan Lei Jincan Lei, Shixian Zhao and Yan Li Shixian Zhao and Yan Li","doi":"10.52568/001189/jcsp/44.06.2022","DOIUrl":"https://doi.org/10.52568/001189/jcsp/44.06.2022","url":null,"abstract":"In this paper, a fast detection method for pesticide residues was proposed, and the qualitative and quantitative detection of the pesticide could be got at once by the method of solution of multiple linear regression equations which were obtained by dual wavelength absorbance and fluorescence spectrometry with least squares method. Moreover, it could detect two kinds of mixed pesticides. Four selected pesticides, aldicarb, fenitrothion, fenvalerate, and chlorothalonil were detected by the method. The results shown that there were good linear relationship in the range of 0.01-1 ppm, and R2 ＞ 0.90. And the method could 100% discriminate the four pesticide residues, the limit of detection was below 8 ppb both single one and mixed one. The recoveries of the pesticides in cabbage samples were observed 92.12%-107.50%. And the recoveries of the mixed pesticides in mineral water samples were observed 86.44%-114.10%. The preliminary study demonstrates that the proposed method has excellent potential application for the safety inspection of food.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70707969","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/000982/jcsp/44.01.2022
Qin Weihan and Yang Yong Qin Weihan and Yang Yong
To derive and verify the chemical structure of the new components in Epimedium, the laws of secondary metabolism and high-resolution mass spectrometry (HRMS) were combined. Based on the chemical literature of Epimedium, the secondary metabolism network of flavonols was constructed, and the possible metabolites were deduced. After the metabolites, information was imported into PeakView software, and the ions with a mass error andlt; 5 ppm, correct isotope distribution, and containing secondary fragments were taken as the target compounds. The chemical structures of new compounds were identified and verified by combining Formula Finder, Mass Calculators, online databases (SciFinder, Reaxys, ChemSpider, etc.) and secondary fragmentation rules. In this study, a total of 4 metabolic pathways and 64 compound structures were deduced, and two new components and 12 new compounds were identified in 54 batches of Epimedium samples from 15 species by high-resolution mass spectrometry. Furthermore, the long and tedious steps of phytochemical separation were simplified, experimental costs were reduced, and a new idea and method were suggested for the analysis and identification of secondary metabolites with pharmacological activity.
{"title":"Identification of New Compounds in Epimedium L. based on Flavonol Secondary Metabolism and High-Resolution Mass Spectrometry","authors":"Qin Weihan and Yang Yong Qin Weihan and Yang Yong","doi":"10.52568/000982/jcsp/44.01.2022","DOIUrl":"https://doi.org/10.52568/000982/jcsp/44.01.2022","url":null,"abstract":"To derive and verify the chemical structure of the new components in Epimedium, the laws of secondary metabolism and high-resolution mass spectrometry (HRMS) were combined. Based on the chemical literature of Epimedium, the secondary metabolism network of flavonols was constructed, and the possible metabolites were deduced. After the metabolites, information was imported into PeakView software, and the ions with a mass error andlt; 5 ppm, correct isotope distribution, and containing secondary fragments were taken as the target compounds. The chemical structures of new compounds were identified and verified by combining Formula Finder, Mass Calculators, online databases (SciFinder, Reaxys, ChemSpider, etc.) and secondary fragmentation rules. In this study, a total of 4 metabolic pathways and 64 compound structures were deduced, and two new components and 12 new compounds were identified in 54 batches of Epimedium samples from 15 species by high-resolution mass spectrometry. Furthermore, the long and tedious steps of phytochemical separation were simplified, experimental costs were reduced, and a new idea and method were suggested for the analysis and identification of secondary metabolites with pharmacological activity.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70706212","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.52568/001068/jcsp/44.04.2022
Senem anl Senem anl, Seyfi Sardogan Seyfi Sardogan, Ay e zdemir and Bar Atalay Ay e zdemir and Bar Atalay
In this study, the dissociation constants of six antidiabetic drugs (rosiglitazon maleate, pioglitazone, glimepride, glibenclamide, gliclazide and glipizide) have been calculated by capillary electrophoresis (CE) technique in water from the mobilities of compounds at several pH values. The dissociation constant values of antidiabetics had been checked with the ones formerly decided withinside the literature and additionally with the statistics expected through the SPARC on-line calculator and ACDLAB. Also, easy, precise, green, accurate and completely validated CE technique for the analysis of glibenclamide in pharmaceutical medicine has been fully developed. The CE technique allowed quantitation over the ranges of 1.00-12.00 μg mL-1. The detection and quantitation limits were determined as 0.036 μg mL-1 and 0.083 μg mL-1 respectively. Rosiglitazone was used as an internal standard and short analysis time (andlt; 3 min.) was observed. The developed capillary electrophoretic technique could be used for ordinary analysis of the glibenclamide and this method can also be used for pharmacokinetic studies.
{"title":"Determination of Pka Values of Antidiabetic Drugs from Mobility Data and Pharmaceutical Analysis by Capillary Electrophoresis","authors":"Senem anl Senem anl, Seyfi Sardogan Seyfi Sardogan, Ay e zdemir and Bar Atalay Ay e zdemir and Bar Atalay","doi":"10.52568/001068/jcsp/44.04.2022","DOIUrl":"https://doi.org/10.52568/001068/jcsp/44.04.2022","url":null,"abstract":"In this study, the dissociation constants of six antidiabetic drugs (rosiglitazon maleate, pioglitazone, glimepride, glibenclamide, gliclazide and glipizide) have been calculated by capillary electrophoresis (CE) technique in water from the mobilities of compounds at several pH values. The dissociation constant values of antidiabetics had been checked with the ones formerly decided withinside the literature and additionally with the statistics expected through the SPARC on-line calculator and ACDLAB. Also, easy, precise, green, accurate and completely validated CE technique for the analysis of glibenclamide in pharmaceutical medicine has been fully developed. The CE technique allowed quantitation over the ranges of 1.00-12.00 μg mL-1. The detection and quantitation limits were determined as 0.036 μg mL-1 and 0.083 μg mL-1 respectively. Rosiglitazone was used as an internal standard and short analysis time (andlt; 3 min.) was observed. The developed capillary electrophoretic technique could be used for ordinary analysis of the glibenclamide and this method can also be used for pharmacokinetic studies.","PeriodicalId":17253,"journal":{"name":"Journal of the chemical society of pakistan","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70707013","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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