Pub Date : 2023-01-01DOI: 10.4236/ajac.2023.1411028
Yun An, Tian Tian, Qinglin Wang, Xingchu Gong, Chenchen Zhang
The purpose of this study was to establish a high-performance liquid chromatography (HPLC) method for the simultaneous determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid in Danhong injection. The chromatographic method employed was as follows: the column was a Welch Ultimate XB-C18 column (250 mm × 4.6 mm, 10 μm), the mobile phase was a gradient elution of 0.4% formic acid aqueous solution (A) and acetonitrile (B), the detection wavelengths were 280 nm for sodium danshensu, protocatechuic aldehyde, and salvianolic acid B and 326 nm for 4-coumaric acid and rosmarinic acid, the sample volume was 10 μL, the flow rate was 1.0 mL/min, and the column temperature was 35°C. This method can realize the separation and determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid within 50 minutes. The linear relationships of the five peak areas and their concentrations are good (R2> 0.9997). The precision RSD values are all less than 1.0%. The reproducibility RSD values are all less than 1.3%. The stability RSD values are all less than 2.2%. The recovery values ranged from 92.4% to 99.4%. This method is simple, accurate, and reproducible. It can be used for the determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid in Danhong injection.
{"title":"A High-Performance Liquid Chromatography Method for the Simultaneous Determination of Five Index Components in Danhong Injection","authors":"Yun An, Tian Tian, Qinglin Wang, Xingchu Gong, Chenchen Zhang","doi":"10.4236/ajac.2023.1411028","DOIUrl":"https://doi.org/10.4236/ajac.2023.1411028","url":null,"abstract":"The purpose of this study was to establish a high-performance liquid chromatography (HPLC) method for the simultaneous determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid in Danhong injection. The chromatographic method employed was as follows: the column was a Welch Ultimate XB-C18 column (250 mm × 4.6 mm, 10 μm), the mobile phase was a gradient elution of 0.4% formic acid aqueous solution (A) and acetonitrile (B), the detection wavelengths were 280 nm for sodium danshensu, protocatechuic aldehyde, and salvianolic acid B and 326 nm for 4-coumaric acid and rosmarinic acid, the sample volume was 10 μL, the flow rate was 1.0 mL/min, and the column temperature was 35°C. This method can realize the separation and determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid within 50 minutes. The linear relationships of the five peak areas and their concentrations are good (R2> 0.9997). The precision RSD values are all less than 1.0%. The reproducibility RSD values are all less than 1.3%. The stability RSD values are all less than 2.2%. The recovery values ranged from 92.4% to 99.4%. This method is simple, accurate, and reproducible. It can be used for the determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid in Danhong injection.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"27 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135260980","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 : 2023-01-01DOI: 10.4236/ajac.2023.149023
Alyssa Beres, Yusuf Yildiz
The iodine value (iodine number) and hydroxyl value are important analytical characteristics of fats and oils. The iodine (I2) required saturating the fatty acids present in 100 grams of the oil or fat. Iodine value is a measure of the total number of double bonds (-C=C-) present in fats and oils. Unsaturated compounds contain molecules with double and triple bonds which are very reactive towards iodine. The iodine value has been determined according to Hanus with iodine monobromide in glacial acetic acid, and then the amount of iodine remaining unreacted is determined by titration using sodium thiosulfate volumetric standard solution. The hydroxyl value is the amount of potassium hydroxide in milligrams that is equivalent to the hydroxyl amount of 1 gram of the sample (mg KOH/g sample). Poloxyl Stearyl Ether is a mixture of the monostearyl ethers of mixed polyethylene glycols. It may contain various amounts of free stearyl alcohol and some free polyethylene glycol. In this study, the iodine value and hydroxyl value have been determined by titration in polyoxyl stearyl ether. Iodine value 1.84 g of I2 absorbed/100g sample, and hydroxyl value 162.65 mg KOH/g sample have been found in poloxyl stearyl ether. The iodine value and hydroxyl value results met the United States Pharmacopeia specifications for Polyoxyl Stearyl Ether.
碘值(碘值)和羟基值是油脂的重要分析特征。碘(I2)需要使100克油或脂肪中的脂肪酸饱和。碘值是脂肪和油中存在的双键(-C=C-)总数的量度。不饱和化合物含有双键和三键的分子，这些分子对碘非常敏感。用一溴化碘在冰醋酸中测定碘值，再用硫代硫酸钠体积标准溶液滴定测定未反应碘量。羟基值是以毫克为单位的氢氧化钾的量，相当于1克样品的羟基量(mg KOH/g样品)。聚氧硬脂基醚是混合聚乙二醇的单硬脂基醚的混合物。它可能含有不同数量的游离硬脂醇和一些游离聚乙二醇。本研究用滴定法测定了聚氧硬脂基醚中的碘值和羟基值。聚氧硬脂基醚的碘值为1.84 g /100g，羟基值为162.65 mg KOH/g。碘值和羟基值符合美国药典对聚氧硬脂基醚的规范。
{"title":"A Comparative Study of the Hydroxyl Value and Iodine Value in Polyoxyl Stearyl Ether in United States Pharmacopeia Specifications","authors":"Alyssa Beres, Yusuf Yildiz","doi":"10.4236/ajac.2023.149023","DOIUrl":"https://doi.org/10.4236/ajac.2023.149023","url":null,"abstract":"The iodine value (iodine number) and hydroxyl value are important analytical characteristics of fats and oils. The iodine (I2) required saturating the fatty acids present in 100 grams of the oil or fat. Iodine value is a measure of the total number of double bonds (-C=C-) present in fats and oils. Unsaturated compounds contain molecules with double and triple bonds which are very reactive towards iodine. The iodine value has been determined according to Hanus with iodine monobromide in glacial acetic acid, and then the amount of iodine remaining unreacted is determined by titration using sodium thiosulfate volumetric standard solution. The hydroxyl value is the amount of potassium hydroxide in milligrams that is equivalent to the hydroxyl amount of 1 gram of the sample (mg KOH/g sample). Poloxyl Stearyl Ether is a mixture of the monostearyl ethers of mixed polyethylene glycols. It may contain various amounts of free stearyl alcohol and some free polyethylene glycol. In this study, the iodine value and hydroxyl value have been determined by titration in polyoxyl stearyl ether. Iodine value 1.84 g of I2 absorbed/100g sample, and hydroxyl value 162.65 mg KOH/g sample have been found in poloxyl stearyl ether. The iodine value and hydroxyl value results met the United States Pharmacopeia specifications for Polyoxyl Stearyl Ether.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"14 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135799369","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 sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM.
{"title":"Determination of Voriconazole in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry: Application in Therapeutic Drug Monitoring","authors":"Waleed Alhussaini, Ezzeldeen Ghanem, Magd Alsahly, Amani Kurdi, Eman Alharbi, Imadul Islam, Majed Aljeraisy","doi":"10.4236/ajac.2023.149021","DOIUrl":"https://doi.org/10.4236/ajac.2023.149021","url":null,"abstract":"A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"65 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135700846","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}
As more and more pollutants threaten human health, it is necessary and essential to develop sensitive, accurate and rapid methods and sensory materials to detect harmful substance. Metal-organic frameworks (MOFs) are inorganic-organic hybrids assembled from inorganic metal ions or clusters and suitable organic ligands. Zinc-based MOFs (Zn-MOFs) have emerged as one of the most promising sensory material of MOFs for practical applications, and attracted significant attention due to structural diversity and incomparable stability properties. However, there are few reviews on systemic summary of synthesis design, mechanism and application of Zn-MOFs. In this review, we summarize the synthesis design methods, structure types and luminescence mechanism of Zn-MOFs sensor recognition in the past ten years and their applications in metal cations, anions, organic compounds and other analytes. Finally, we present a short conclusion, and look forward to the future development direction of Zn-MOFs.
{"title":"Recent Progress in Synthesis, Mechanism and Applications of Zinc-Based Metal-Organic Frameworks for Fluorescent Sensing","authors":"Xiaojing Mao, Huachang Li, Jiemin Liu, Yehong Shi, Lijun Kuai","doi":"10.4236/ajac.2023.149022","DOIUrl":"https://doi.org/10.4236/ajac.2023.149022","url":null,"abstract":"As more and more pollutants threaten human health, it is necessary and essential to develop sensitive, accurate and rapid methods and sensory materials to detect harmful substance. Metal-organic frameworks (MOFs) are inorganic-organic hybrids assembled from inorganic metal ions or clusters and suitable organic ligands. Zinc-based MOFs (Zn-MOFs) have emerged as one of the most promising sensory material of MOFs for practical applications, and attracted significant attention due to structural diversity and incomparable stability properties. However, there are few reviews on systemic summary of synthesis design, mechanism and application of Zn-MOFs. In this review, we summarize the synthesis design methods, structure types and luminescence mechanism of Zn-MOFs sensor recognition in the past ten years and their applications in metal cations, anions, organic compounds and other analytes. Finally, we present a short conclusion, and look forward to the future development direction of Zn-MOFs.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"36 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135701168","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 : 2023-01-01DOI: 10.4236/ajac.2023.149020
Martin Nduka Nwanekezie, Samuel Enoroghoe Ogbeide, Nwosu Cynthia Chidiebere, Godspower O. Sebe
This research investigates the efficacy of activated Gmelina Wood Sawdust (GWS) as an adsorbent for the removal of methylene blue (MB) dye from aqueous solutions, in comparison with raw GWS. The study employs laboratory experiments to assess the percentage of dye removal across various temperature and pH conditions. The adsorption process is scrutinized under different parameters, encompassing contact time, initial dye concentration, adsorbent dosage, temperature, and pH. Results demonstrate that activated GWS surpasses its raw counterpart, showcasing superior MB dye removal percentages. Extended contact times increased initial dye concentrations, and higher adsorbent dosages contribute positively to removal efficiency, while temperature exhibits an inverse relationship with dye removal. Optimal adsorption occurs at a pH of 7.0, aligning with the adsorbent’s zero-point charge (pHzpc), underscoring the role of surface charge in the adsorption process. This study underscores the potential of activated GWS as an economical and promising adsorbent material for addressing pollutants. Furthermore, the utilization of activated carbon derived from abundant agricultural waste underscores an environmentally conscious approach to adsorption applications. The ability to tailor the size and properties of activated carbon particles opens avenues for optimizing adsorption capabilities, thereby presenting opportunities for enhanced water treatment solutions.
{"title":"Optimizing Methylene Blue Removal from Textile Effluents: Comparative Study of Adsorption Efficiency Using Raw and Activated Carbon Derived from <i>Gmelina</i> Wood Wastes","authors":"Martin Nduka Nwanekezie, Samuel Enoroghoe Ogbeide, Nwosu Cynthia Chidiebere, Godspower O. Sebe","doi":"10.4236/ajac.2023.149020","DOIUrl":"https://doi.org/10.4236/ajac.2023.149020","url":null,"abstract":"This research investigates the efficacy of activated Gmelina Wood Sawdust (GWS) as an adsorbent for the removal of methylene blue (MB) dye from aqueous solutions, in comparison with raw GWS. The study employs laboratory experiments to assess the percentage of dye removal across various temperature and pH conditions. The adsorption process is scrutinized under different parameters, encompassing contact time, initial dye concentration, adsorbent dosage, temperature, and pH. Results demonstrate that activated GWS surpasses its raw counterpart, showcasing superior MB dye removal percentages. Extended contact times increased initial dye concentrations, and higher adsorbent dosages contribute positively to removal efficiency, while temperature exhibits an inverse relationship with dye removal. Optimal adsorption occurs at a pH of 7.0, aligning with the adsorbent’s zero-point charge (pHzpc), underscoring the role of surface charge in the adsorption process. This study underscores the potential of activated GWS as an economical and promising adsorbent material for addressing pollutants. Furthermore, the utilization of activated carbon derived from abundant agricultural waste underscores an environmentally conscious approach to adsorption applications. The ability to tailor the size and properties of activated carbon particles opens avenues for optimizing adsorption capabilities, thereby presenting opportunities for enhanced water treatment solutions.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"275 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135651056","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 : 2023-01-01DOI: 10.4236/ajac.2023.1410026
Boyu Zhang, Kuo Zhang, Ziqiang Duan, Jianping Zhu, Junan Gao
{"title":"Y Zeolites Modified by Organosilane for Toluene Adsorption under High Humidity Condition","authors":"Boyu Zhang, Kuo Zhang, Ziqiang Duan, Jianping Zhu, Junan Gao","doi":"10.4236/ajac.2023.1410026","DOIUrl":"https://doi.org/10.4236/ajac.2023.1410026","url":null,"abstract":"","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"17 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135316707","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}
Amino acids are very important compounds for the body and are involved in important functions that keep us healthy. Amino acids are essential components such as valine, proline, glutamine and glutamic acid. They can be synthesized either naturally or artificially. To examine the metabolism and regulate the synthesis process, compounds labeled with nitrogen or carbon isotopes need to be used. These isotopic compounds allow for more extensive research and enable studies that would otherwise be impossible. However, their use is dependent on the availability of simple, efficient methods for isotopic analysis. Currently, the determination of the atomic fraction of carbon and nitrogen isotopes is only possible through their conversion into molecular nitrogen or carbon monoxide or carbon dioxide. This leads to the loss of information about isotopic enrichment in specific centers of the molecule. This article explores a new direct approach to determining the atomic fraction of carbon and nitrogen isotopes in the isotope-modified or identical centers of these compounds. This method eliminates the transfer process and dilution due to nitrogen and carbon impurities. It is now possible to simultaneously determine the atomic fraction of nitrogen and carbon isotopes in the research substance. This method can be applied to amino acids, making it an effective tool for proposing new research methods. Several articles [1] [2] [3] have proposed similar methods for organic compounds and amino acids.
{"title":"Methods for the Determination of Stable Isotopes of Carbon and Nitrogen Directly in Valine, Proline, Glutamine, and Glutamic Acid","authors":"Lamzira Farulava, Levani Eliashvili, Vakhtang Betlemidze, Bachana Sulava","doi":"10.4236/ajac.2023.1410027","DOIUrl":"https://doi.org/10.4236/ajac.2023.1410027","url":null,"abstract":"Amino acids are very important compounds for the body and are involved in important functions that keep us healthy. Amino acids are essential components such as valine, proline, glutamine and glutamic acid. They can be synthesized either naturally or artificially. To examine the metabolism and regulate the synthesis process, compounds labeled with nitrogen or carbon isotopes need to be used. These isotopic compounds allow for more extensive research and enable studies that would otherwise be impossible. However, their use is dependent on the availability of simple, efficient methods for isotopic analysis. Currently, the determination of the atomic fraction of carbon and nitrogen isotopes is only possible through their conversion into molecular nitrogen or carbon monoxide or carbon dioxide. This leads to the loss of information about isotopic enrichment in specific centers of the molecule. This article explores a new direct approach to determining the atomic fraction of carbon and nitrogen isotopes in the isotope-modified or identical centers of these compounds. This method eliminates the transfer process and dilution due to nitrogen and carbon impurities. It is now possible to simultaneously determine the atomic fraction of nitrogen and carbon isotopes in the research substance. This method can be applied to amino acids, making it an effective tool for proposing new research methods. Several articles [1] [2] [3] have proposed similar methods for organic compounds and amino acids.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"8 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135262160","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}
Non-compliant antibiotics pose problems of therapeutic efficacy at the level of the individual, but also a serious public health problem. The objective of our study was to evaluate the quality of generic amoxicillin (42 samples) by analytical methods in Dakar/Senegal. At 100% visual inspection of compliance; 100% compliance uniformity test; at the dissolution test all > 80% (86.8% to 108.8%). The presence of amoxicillin with the following contents: Tablets (95.2% to 104.1%); Capsules (91.5% to 113.9%) and Suspensions drinkable (96.9% - 118.7%). All the samples in our study are 100% compliant according to the European and American pharmacopoeias (90% - 120%). Other studies should therefore be oriented in the direction of stability as well as the dosage of degradation products.
{"title":"Audit of the Physico-Chemical Quality of Amoxicillin Based Drugs Marketed in Senegal","authors":"Coulibaly Dalané Bernadette, Sow Fatoumata Tata, Naco Mohamed El Béchir, N’Diaye Mahamar, Toure Hamadoun Abba, Mariko Madani, Dackouo Blaise, Diouf Diéry, Koumare Benoit Yaranga, Sarr Serigne Omar","doi":"10.4236/ajac.2023.149019","DOIUrl":"https://doi.org/10.4236/ajac.2023.149019","url":null,"abstract":"Non-compliant antibiotics pose problems of therapeutic efficacy at the level of the individual, but also a serious public health problem. The objective of our study was to evaluate the quality of generic amoxicillin (42 samples) by analytical methods in Dakar/Senegal. At 100% visual inspection of compliance; 100% compliance uniformity test; at the dissolution test all > 80% (86.8% to 108.8%). The presence of amoxicillin with the following contents: Tablets (95.2% to 104.1%); Capsules (91.5% to 113.9%) and Suspensions drinkable (96.9% - 118.7%). All the samples in our study are 100% compliant according to the European and American pharmacopoeias (90% - 120%). Other studies should therefore be oriented in the direction of stability as well as the dosage of degradation products.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"127 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135651062","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 : 2023-01-01DOI: 10.4236/ajac.2023.1410024
Huan Yao, Siqi Zeng, Xianghua Wang, Hang Li, Bing Du
Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS for the simultaneous quantification of 2 and 3-MCPD esters in infant milk powder and edible vegetable oils. The developed protocol included fat fraction in infant milk powder and edible vegetable oils samples was extracted and treated with sodium methylate-methanol to cleave the ester bonds of the 2- and 3-MCPD esters, moreover, standard samples of deuterium isotope-labeled 2- and 3-MCPD palmitic acid double esters and stearic acid double esters were used as the internal standards. Furthermore, this method was validated when it was applied to food products, concrete manifestation in its good accuracy (the recovery of MCPD esters ranged from 86% to 114%), high sensitivity (the LOD of 3-MCPD and 2-MCPD esters were 0.025 and 0.020 mg/kg, LOQ were 0.075, 0.060 mg/kg, respectively) and satisfactory repeatability (RSD below 6.8%) for all analytes. In the 150 commercial edible vegetable oils and infant formula milk powder samples, we obtained a preliminary profile of MCPD ester contamination.
{"title":"Simultaneous Determination of 2- and 3-MCPD Esters in Infant Formula Milk Powder and Edible Vegetable Oils by Gas Chromatography-Mass Spectrometry","authors":"Huan Yao, Siqi Zeng, Xianghua Wang, Hang Li, Bing Du","doi":"10.4236/ajac.2023.1410024","DOIUrl":"https://doi.org/10.4236/ajac.2023.1410024","url":null,"abstract":"Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS for the simultaneous quantification of 2 and 3-MCPD esters in infant milk powder and edible vegetable oils. The developed protocol included fat fraction in infant milk powder and edible vegetable oils samples was extracted and treated with sodium methylate-methanol to cleave the ester bonds of the 2- and 3-MCPD esters, moreover, standard samples of deuterium isotope-labeled 2- and 3-MCPD palmitic acid double esters and stearic acid double esters were used as the internal standards. Furthermore, this method was validated when it was applied to food products, concrete manifestation in its good accuracy (the recovery of MCPD esters ranged from 86% to 114%), high sensitivity (the LOD of 3-MCPD and 2-MCPD esters were 0.025 and 0.020 mg/kg, LOQ were 0.075, 0.060 mg/kg, respectively) and satisfactory repeatability (RSD below 6.8%) for all analytes. In the 150 commercial edible vegetable oils and infant formula milk powder samples, we obtained a preliminary profile of MCPD ester contamination.","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"71 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135009990","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}
Capillary zone electrophoresis (CZE) is a sensitive and rapid technique for determining traces of inorganic cations in water samples. CZE with indirect UV-diode array detection (CZE-DAD) was utilized to identify several inorganic cations in natural, potable, and wastewater samples. A pH 4.35 background electrolyte system was employed and consisted of 15 mM imidazole, 8 mM malonic acid, 2 mM 18-crown-6 ether as complexing agents, 10% v/v methanol as an organic modifier with indirect absorbance reference at 214 nm. The CZE method involved electromigration injection at 5 kV for 5 s, a separation voltage of 20 kV at 25°C, and a detection wavelength of 280 nm. Six main cations (ammonium [Formula: see text], potassium K+, calcium Ca2+, sodium Na+, magnesium Mg2+, and lead Pb2+) were tested, and all but lead, were detected in the water samples at concentrations between 0.03 and 755 ppm with a detection limit ranging between 0.023 and 0.084 ppm. The successful evaluation of the proposed methodology allowed us to reliably detect and separate six metal ions in different water samples without any pretreatment. All water samples were collected from Northern New York towns and the Raquette River water system, the third longest river in New York State and the largest watershed of the central and western Adirondacks.
{"title":"Detection and Separation of Inorganic Cations in Natural, Potable, and Wastewater Samples Using Capillary Zone Electrophoresis with Indirect UV Detection.","authors":"Lara Varden, Fadi Bou-Abdallah","doi":"10.4236/ajac.2017.81007","DOIUrl":"https://doi.org/10.4236/ajac.2017.81007","url":null,"abstract":"<p><p>Capillary zone electrophoresis (CZE) is a sensitive and rapid technique for determining traces of inorganic cations in water samples. CZE with indirect UV-diode array detection (CZE-DAD) was utilized to identify several inorganic cations in natural, potable, and wastewater samples. A pH 4.35 background electrolyte system was employed and consisted of 15 mM imidazole, 8 mM malonic acid, 2 mM 18-crown-6 ether as complexing agents, 10% v/v methanol as an organic modifier with indirect absorbance reference at 214 nm. The CZE method involved electromigration injection at 5 kV for 5 s, a separation voltage of 20 kV at 25°C, and a detection wavelength of 280 nm. Six main cations (ammonium [Formula: see text], potassium K<sup>+</sup>, calcium Ca<sup>2+</sup>, sodium Na<sup>+</sup>, magnesium Mg<sup>2+</sup>, and lead Pb<sup>2+</sup>) were tested, and all but lead, were detected in the water samples at concentrations between 0.03 and 755 ppm with a detection limit ranging between 0.023 and 0.084 ppm. The successful evaluation of the proposed methodology allowed us to reliably detect and separate six metal ions in different water samples without any pretreatment. All water samples were collected from Northern New York towns and the Raquette River water system, the third longest river in New York State and the largest watershed of the central and western Adirondacks.</p>","PeriodicalId":7477,"journal":{"name":"American Journal of Analytical Chemistry","volume":"8 1","pages":"81-94"},"PeriodicalIF":0.0,"publicationDate":"2017-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4236/ajac.2017.81007","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"35630517","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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