Samples from petroleum contaminated soil Eleme, Port Harcourt and from non petroleum contaminated soil, Awka, Nigeria serving as control were analyzed for heavy metals. The results of the analysis showed that the metals concentrations in mg/kg were Ni<0.05- 2.05, Cr 0.005 -0.37, Cd<0.005 - 0.008, Zn 0.14 -2.87 Pb<0.02- 0.19 Fe 12.32-29.11 ,Mn< 0.008- 0.036, Se<0.001, As<0.001, and V<0.001. Majority of the metal concentrations were above those of the control. Though the values obtained did not exceed soil quality standards stipulated in the Environmental Management Regulations, 2007, the toxic metals could accumulate to a threatening level over a period of time. Food poisoning, occupational hazards and various disorders emanate from heavy load of toxic metals in our environment.
{"title":"Assessment Of Some Heavy Metals As Contaminants In Petroleum Contaminated Soils Of Eleme, Port Harcourt Nigeria","authors":"U. Ojukwu, A. Eboatu","doi":"10.5281/ZENODO.5335980","DOIUrl":"https://doi.org/10.5281/ZENODO.5335980","url":null,"abstract":"Samples from petroleum contaminated soil Eleme, Port Harcourt and from non petroleum contaminated soil, Awka, Nigeria serving as control were analyzed for heavy metals. The results of the analysis showed that the metals concentrations in mg/kg were Ni<0.05- 2.05, Cr 0.005 -0.37, Cd<0.005 - 0.008, Zn 0.14 -2.87 Pb<0.02- 0.19 Fe 12.32-29.11 ,Mn< 0.008- 0.036, Se<0.001, As<0.001, and V<0.001. \u0000Majority of the metal concentrations were above those of the control. Though the values obtained did not exceed soil quality standards stipulated in the Environmental Management Regulations, 2007, the toxic metals could accumulate to a threatening level over a period of time. Food poisoning, occupational hazards and various disorders emanate from heavy load of toxic metals in our environment.","PeriodicalId":7823,"journal":{"name":"Analytical chemistry, an Indian journal","volume":"50 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88965882","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}
Simple, accurate, sensitive and validated UV stability-indicating spectrophotometric and chemometric methods were developed for determination of CitalopramHydrobromide (CT) in presence of its alkaline, oxidative degradation products and in its pharmaceutical preparation. Method (A) is a successive derivative ratio spectrophotometricone, which depends on the successive derivative of ratio spectra in two steps andmeasuring Citalopram Hydrobromide at 277nmand 293nm.Method (B) ismean centering of ratio spectra which dependson using the mean centered ratio spectra in two successive steps and measuring the mean centeredvalues of the second ratio spectra at 237nm and method (C) used two chemometric techniques ; principal component regression(PCR) and partial least-squares (PLS). The proposed methods werechecked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceuticalformulation containing Citalopram Hydrobromide. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically comparedwith those obtained froma compendialHPLCmethod, showing no significant difference with respect to accuracy and precision.
{"title":"Quantitative determination of citalopramhydrobromide by spectrophotometry and chemometry in presence of its degradation productsand additives in pharmaceutical preparation","authors":"HeshamSalem, MarianneNebsen","doi":"10.15242/iicbe.c0715105","DOIUrl":"https://doi.org/10.15242/iicbe.c0715105","url":null,"abstract":"Simple, accurate, sensitive and validated UV stability-indicating spectrophotometric and chemometric methods were developed for determination of CitalopramHydrobromide (CT) in presence of its alkaline, oxidative degradation products and in its pharmaceutical preparation. Method (A) is a successive derivative ratio spectrophotometricone, which depends on the successive derivative of ratio spectra in two steps andmeasuring Citalopram Hydrobromide at 277nmand 293nm.Method (B) ismean centering of ratio spectra which dependson using the mean centered ratio spectra in two successive steps and measuring the mean centeredvalues of the second ratio spectra at 237nm and method (C) used two chemometric techniques ; principal component regression(PCR) and partial least-squares (PLS). The proposed methods werechecked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceuticalformulation containing Citalopram Hydrobromide. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically comparedwith those obtained froma compendialHPLCmethod, showing no significant difference with respect to accuracy and precision.","PeriodicalId":7823,"journal":{"name":"Analytical chemistry, an Indian journal","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2016-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76745241","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}
Pub Date : 2012-08-31DOI: 10.5923/j.fs.20120202.01
R.S.Lokh, P.U.Singare, P. Jadhav
Related substances by HPLC method was developed and validated for Diphenoxylate hydrochloride bulk drug and its three potential impurities i.e. Diphenoxylic acid (degradation product), Nitrile amide (precursor) and Bromo Diphenyl butro nitrile (precursor). Analysis was performed on AGILENT 1100 SERIES HPLC system with auto injector and binary gradient high pressure mixing pump on Inersil ODS-3 (RP C 18) column. Mobile phase of Acetonitrile and HPLC water pH adjusted to 2.3 with orthophosphoric acid in the ratio of 25:75 (v/v) with change in the ratio of mobile phase by linear gradient to 85: 25 (v/v) in 45 minute was pumped at 2mL/min and the detection was done at 210 nm. The parameter for which the method was validated included specificity, limit of detection and quantitation, linearity, precision, accuracy and robustness. The method was successfully used to quantitate the levels known impurities {i.e. Diphenoxylic acid (degradation product), Nitrileamide (precursor) and Bromo Diphenyl butro nitrile (precursor)} and unkown impurities in Diphenoxylate hydro- chloride bulk drug.
{"title":"Development and validation for reverse phase high performance liquid chromatographic method for simultaneously determination for diphenoxylic acid, nitrileamide and bromdiphenyl butoro nitrile in diphenoxylate hydrochloride bulk drug","authors":"R.S.Lokh, P.U.Singare, P. Jadhav","doi":"10.5923/j.fs.20120202.01","DOIUrl":"https://doi.org/10.5923/j.fs.20120202.01","url":null,"abstract":"Related substances by HPLC method was developed and validated for Diphenoxylate hydrochloride bulk drug and its three potential impurities i.e. Diphenoxylic acid (degradation product), Nitrile amide (precursor) and Bromo Diphenyl butro nitrile (precursor). Analysis was performed on AGILENT 1100 SERIES HPLC system with auto injector and binary gradient high pressure mixing pump on Inersil ODS-3 (RP C 18) column. Mobile phase of Acetonitrile and HPLC water pH adjusted to 2.3 with orthophosphoric acid in the ratio of 25:75 (v/v) with change in the ratio of mobile phase by linear gradient to 85: 25 (v/v) in 45 minute was pumped at 2mL/min and the detection was done at 210 nm. The parameter for which the method was validated included specificity, limit of detection and quantitation, linearity, precision, accuracy and robustness. The method was successfully used to quantitate the levels known impurities {i.e. Diphenoxylic acid (degradation product), Nitrileamide (precursor) and Bromo Diphenyl butro nitrile (precursor)} and unkown impurities in Diphenoxylate hydro- chloride bulk drug.","PeriodicalId":7823,"journal":{"name":"Analytical chemistry, an Indian journal","volume":"18 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2012-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81172143","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}
Pub Date : 2012-01-01DOI: 10.1007/978-90-481-8650-1_13
S. R. Phule, H. Aher, S. Lawande, S. Kuchekar
{"title":"Reverse Phase Extraction Chromatographic Separation of Trivalent Bismuth Using Liquid Anion Exchanger","authors":"S. R. Phule, H. Aher, S. Lawande, S. Kuchekar","doi":"10.1007/978-90-481-8650-1_13","DOIUrl":"https://doi.org/10.1007/978-90-481-8650-1_13","url":null,"abstract":"","PeriodicalId":7823,"journal":{"name":"Analytical chemistry, an Indian journal","volume":"50 1","pages":"209-217"},"PeriodicalIF":0.0,"publicationDate":"2012-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85749177","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}
Anew, rapid and sensitive reverse phase HPLC method was developed and validated for the determination of benzhexol hydrochloride in tablet formulations and urine. The mobile phase used acetonitrile and water, (50 %v/v) adjust pH to 5 using phosphoric acid. The separation was achieved on C18 reversed-phase column (250 mmi´4 mmi.d.). The flowrate was 0.6 ml/min and UV detection at 254nm. The retention time for benzhexol hydrochloride was 7.4 min. The calibration curve was linear up to 40iÂg/mL. The mean recovery for benzhexol hydrochloride is 101.16. The assaywas precisewithin day and between days. The method provided excellent sensitivity, recovery, accuracy and reproducibility in therapeutic or toxic concentrations. Common excipients do not interfere.
建立了一种快速、灵敏的反相高效液相色谱法测定盐酸苯甲索片剂和尿液中的含量。流动相为乙腈和水，(50% v/v)用磷酸调节pH至5。在C18反相柱(250 mmi´4 mm .d.)上进行分离。流速0.6 ml/min，紫外检测波长254nm。盐酸苯甲索的保留时间为7.4 min。校准曲线在40i μ -g /mL范围内呈线性。盐酸苯哲索的平均回收率为101.16。白天和白天之间的测定都很精确。该方法在治疗浓度或毒性浓度下均具有良好的灵敏度、回收率、准确性和重现性。普通赋形剂不干扰。
{"title":"RP HPLC determination of benzhexol hydrochloride in tablet formulations and urine","authors":"R. Farag, Ashraf M. Ahmed","doi":"10.21608/ABSB.2010.7380","DOIUrl":"https://doi.org/10.21608/ABSB.2010.7380","url":null,"abstract":"Anew, rapid and sensitive reverse phase HPLC method was developed and validated for the determination of benzhexol hydrochloride in tablet formulations and urine. The mobile phase used acetonitrile and water, (50 %v/v) adjust pH to 5 using phosphoric acid. The separation was achieved on C18 reversed-phase column (250 mmi´4 mmi.d.). The flowrate was 0.6 ml/min and UV detection at 254nm. The retention time for benzhexol hydrochloride was 7.4 min. The calibration curve was linear up to 40iÂg/mL. The mean recovery for benzhexol hydrochloride is 101.16. The assaywas precisewithin day and between days. The method provided excellent sensitivity, recovery, accuracy and reproducibility in therapeutic or toxic concentrations. Common excipients do not interfere.","PeriodicalId":7823,"journal":{"name":"Analytical chemistry, an Indian journal","volume":"57 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2010-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80224487","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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