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An Analytical Procedure by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) for the Quantitation of Total Phosphorus Content on the Surface of the Manufacturing Equipment for Oligonucleotides
Daisuke Furukawa,
Masami Nakai,
Masato Kazusaki
Issue:
Volume 8, Issue 1, March 2020
Pages:
1-4
Received:
25 December 2019
Accepted:
7 January 2020
Published:
30 January 2020
Abstract: An analytical procedure by the inductively coupled plasma mass spectrometry (ICP-MS) is provided to quantitate the remaining phosphorus amount on the surface of the manufacturing equipment for the oligonucleotide active pharmaceutical ingredient (API). In this analytical procedure, the sample solutions obtained from the rinse sampling and direct surface sampling methods are directly injected into the ICP-MS equipment without the inspissation of the extraction liquid. The limit of quantitation for phosphorous was 0.02 µg/mL. Quantitation of phosphorous was achieved over a linear range of 0.02 to 0.8 µg/mL. Analytical validation was carried out to prove that this analytical procedure is appropriate and effective to monitor the cleanliness of the manufacturing equipment after the oligonucleotide API manufacturing and the following cleaning of the equipment. Calibration curve originally passed through the origin with correlation coefficient of 0.999. The precision through the rinse sampling method was within ±10%. The satisfactory accuracy for the rinse sampling method was proven from the assessment of linearity and precision. The precision and accuracy of the analytical procedure were both within ±10% for the direct surface sampling method. The described analytical procedure by ICP-MS following the two types of the sampling procedures can easily be applied to the routine analysis for the verification of the cleanliness of the manufacturing equipment for oligonucleotide API.
Abstract: An analytical procedure by the inductively coupled plasma mass spectrometry (ICP-MS) is provided to quantitate the remaining phosphorus amount on the surface of the manufacturing equipment for the oligonucleotide active pharmaceutical ingredient (API). In this analytical procedure, the sample solutions obtained from the rinse sampling and direct su...
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Analysis of Organic Components by DLLME Based on the Solidification of a Floating Organic Droplet Followed with GC/MS in Wood Vinegar
Qiang Sun,
Yuliang Gao,
Liyan Wang
Issue:
Volume 8, Issue 1, March 2020
Pages:
5-11
Received:
21 December 2019
Accepted:
8 January 2020
Published:
31 January 2020
Abstract: A simple, efficient and environmentally friendly method has been established for the analysis of organic components in wood vinegar (WV) by dispersive liquid-liquid micro-extraction based on solidification of floating organic droplet (DLLME-SFO) coupled with GC/MS. Several variables that affect the extraction efficiency, including the type and volume of the extractant and dispersant, extraction time and the mass fraction of sodium chloride were optimized. Under the optimum conditions, the sample extracted were analyzed by GC/MS. The result shows that, apart from the main component of acetic acid, many kinds of ketone compound, phenol compound, ester compound, aldehyde and alcohol compound exist in the WV. The proposed method has been successfully employed to determine the organic components in the WV.
Abstract: A simple, efficient and environmentally friendly method has been established for the analysis of organic components in wood vinegar (WV) by dispersive liquid-liquid micro-extraction based on solidification of floating organic droplet (DLLME-SFO) coupled with GC/MS. Several variables that affect the extraction efficiency, including the type and volu...
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LC/MS Analysis of Cyclo Fatty Acid-containing Triacylglycerols in Cottonseed Oil
Shuji Hirayama,
Daichi Shinozaki,
Yoshiya Izumi
Issue:
Volume 8, Issue 1, March 2020
Pages:
12-17
Received:
22 December 2019
Accepted:
15 January 2020
Published:
31 January 2020
Abstract: We measured the constituent triacylglycerol of cotton oil, the only edible oil containing a cyclo fatty acid. Due to the difficulty of obtaining a standard for triacylglycerols containing cyclo fatty acids, cotton oil is analyzed using cyclo triacylglycerol in kapok oil as a reference. Analytical methods used liquid chromatography fast atom bombardment mass spectrometry (LC / FAB-MS) using a matrix of 3% m-NBA containing 3 mM NaCl, and orthogonal transfer method for APCI / TOF-MS. FAB mass spectral properties of triacylglycerols containing cyclo fatty acids can be observed with [M + Na]+, [M-1]+ molecular ions, and [M- (RCOO)] + fragments. In the orthogonal APCI / TOF-MS spectrum, only the [M-1] + molecular ion appears, so that the presence of triacylglycerol containing CPFA becomes apparent. On the other hand, chain triacylglycerol can be observed as [M + 1]+ molecular ions and [M- (RCOO)]+ fragments. Based on these observations, triacylglycerols containing ten types of cyclo fatty acids were successfully successfully detected in crude cottonseed oil. In addition, the APCI/TOF-MS technique successfully detected dilinoleoyl-marvalyl-glycerol and palmtoyl-linoleoyl-marvalyl glycerol in the purified cottonseed oil.
Abstract: We measured the constituent triacylglycerol of cotton oil, the only edible oil containing a cyclo fatty acid. Due to the difficulty of obtaining a standard for triacylglycerols containing cyclo fatty acids, cotton oil is analyzed using cyclo triacylglycerol in kapok oil as a reference. Analytical methods used liquid chromatography fast atom bombard...
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Fatty Amides in Minutes: Direct Formation from Fatty Esters in a Green Synthetic Process
Onyanobi Abel-Anyebe,
Nabil Idris,
Djene Keita,
Kieran Ita Ekpenyong,
Momoh Audu Yakubu
Issue:
Volume 8, Issue 1, March 2020
Pages:
18-28
Received:
25 July 2019
Accepted:
20 August 2019
Published:
13 February 2020
Abstract: Fatty amides are used in the manufacture of drugs, cosmetics, plastics, insecticides, etc. but the synthetic process involves fatty ester-derived fatty acid steps with economic and environmental consequences. Fatty esters (vegetable oils) are available in abundance and renewable but have not been used directly or cost effectively in the production of fatty amides. The fatty ester is usually first stripped to fatty acids resulting in a two-step instead of a single step synthesis which requires high temperatures (100 – 240°C), long reaction time (3 – 72 hours) and the use of catalyst. We had previously reported on a novel green method for the direct formation of fatty amides from a fatty ester. In the present study, the functionality and applicability of this green method is evaluated using a culinary and non-culinary oil namely peanut and castor oils. Each oil sample was hydrolyzed with NaOH in a non-aqueous medium and reacted in-situ with NH4Cl at 50°C in a reaction time of 60 minutes with no catalyst added. Conversions of 83 and 79% were recorded for the reactions of peanut and castor oils, respectively. The products of synthesis were characterized by Fourier-transform infrared spectroscopy (FT-IR) and various concentrations of product samples and two reference samples - erucamide and oleamide obtained from Sigma Aldrich - were subjected to Gas chromatography – Mass spectrometry (GC/MS) analysis. The qualitative GC-MS reports revealed the presence of 9-octadecenamide (oleamide) and hexadecanamide (palmitamide) at retention times of 27.76 and 23.90 minutes, respectively for all samples, including the reference. The predominant component of the second reference sample, erucamide, was found to be 13-docosenamide (erucamide) appearing at GC retention time of 32.58 minutes. The IR spectra of the products are strongly indicative of the presence of amides. The GC-MS analysis of the product samples confirms the formation of fatty amides. The detection of oleamide and erucamide in the reference samples and the detection of methyl ricinoleate at GC retention time of 26.573 minutes in the castor oil product sample validates the GC-MS analysis and confirms the functionality and applicability of this novel method of synthesis.
Abstract: Fatty amides are used in the manufacture of drugs, cosmetics, plastics, insecticides, etc. but the synthetic process involves fatty ester-derived fatty acid steps with economic and environmental consequences. Fatty esters (vegetable oils) are available in abundance and renewable but have not been used directly or cost effectively in the production ...
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Glycemic Index of Traditional Meal (Dambu) from Pearl Millet and Maize
Maimuna Ladidi Aliyu,
Safiya Aliyu Tijjani,
Danladi Amodu Ameh,
Aisha Babagana
Issue:
Volume 8, Issue 1, March 2020
Pages:
29-32
Received:
13 February 2020
Accepted:
25 February 2020
Published:
10 March 2020
Abstract: The aim of this study is to determine the blood glucose response of traditionally prepared meal called Dambu from millet and maize enriched with beans, groundnut and vegetables. The cereals grains and other ingredients were purchased from a local market in Kaduna metropolis, and the preparation of the meal, blood glucose response with glycemic index method of determination used followed standard procedures. Result obtained indicated that product (Dambu) made from maize had higher (5.2±0.8) blood glucose response among female subjects, while lowest (5.14±0.53) blood glucose response value was recorded in subjects fed with product from millet. For the male subjects, the product made from millet had higher (4.94±0.9) blood glucose response was recorded in subjects fed with products (Dambu) from maize. Both male and female subjects fed with product (Dambu) from maize had the lowest (41.51%) and (40.33%) glycemic index respectively. T-test was used to assess the sensory attributes of the products and the products were significantly different (p<0.05). The product (Dambu) from millet can be used for the management and control of diabetes as it showed low glycemic index and can also be used as healthy meal. Dambu from maize had the overall acceptability in flavor, taste, texture and colour, and it was the most preferred than Dambu from millet.
Abstract: The aim of this study is to determine the blood glucose response of traditionally prepared meal called Dambu from millet and maize enriched with beans, groundnut and vegetables. The cereals grains and other ingredients were purchased from a local market in Kaduna metropolis, and the preparation of the meal, blood glucose response with glycemic inde...
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Standardisation Process of Saye, a Traditional Polyherbal Formulation Remedy for Malaria: Physico-chemical Analysis and Phytochemical Investigation
Jules Yoda,
Jean Claude Ouedraogo,
Salfo Ouedraogo,
Maminata Traore-Coulibaly,
Felix Kini,
Marius Lompo,
Sylvin Ouedraogo
Issue:
Volume 8, Issue 1, March 2020
Pages:
33-40
Received:
18 February 2020
Accepted:
3 March 2020
Published:
10 March 2020
Abstract: The use of herbal drugs for primary care is nowadays central to the global health system. In developing countries, it meets both economic and socio-cultural requirements. However, this increase about the use of herbal medicines has led to various forms of abuses related to factors that are generally extrinsic to the drug, such as incorrect botanical identification, falsification, fungal or bacterial contamination, etc. The need for the standardization of herbal drugs is more than ever important for the viability of phytotherapy. This study focuses on saye, a mixture of three plants including the root of Cochlospermum planchonii; the whole plant of Phyllanthus amarus and the leaves of Cassia alata. This traditional polyherbal formulation that we intend to promote is used in Burkina Faso as a herbal tea to treat malaria. In this present study, the aim is to control the quality and standardization of the saye and its different components in order to produce an antimalarial phytomedicine. More precisely, we present here, the phytochemical composition and physico-chemical study of the mixture and the vegetable raw materials. In this study, we are particularly concerned with the study of organoleptic properties, moisture content, total ash content, successive extraction yields, fingerprinting by thin layer chromatography, phytochemical screening and total flavonoids content. To evaluate the content of flavonoids selected as chemical bioactive marker, we used a method of spectrophotometric assay. The phytochemical study established fingerprints, identified the main secondary metabolites and determined the total flavonoid content in a selective extract of the saye. The physico-chemical analysis provided satisfactory results on the main indices, such as moisture content, total ash, heavy metals, etc. These results indicate a good treatment of plant raw materials and will certainly be used for the standardization of the drug and its quality control for future clinical studies.
Abstract: The use of herbal drugs for primary care is nowadays central to the global health system. In developing countries, it meets both economic and socio-cultural requirements. However, this increase about the use of herbal medicines has led to various forms of abuses related to factors that are generally extrinsic to the drug, such as incorrect botanica...
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