1H-NMR spectroscopic quantitative determination of clobazam

The 1H-NMR spectrum of clobazam showed a sharp singlet at 3.49 ppm assigned for the N-CH3, which was chosen for the quantitative measurements. The method involves comparing the integral of this signal to that of a sharp singlet at sigma 6.41 ppm assigned for maleic acid, used as internal standard for comparison. A standard curve was plotted the integration ratio Ic/Im and the amount of clobazam in mg. Good results were obtained on application of this method on authentic sample of clobazam. The mean percentage recovery is 100.12 +/- 1.133. Good recoveries were also obtained on application of this method on tablet form [Frisium] using standard addition technique. The mean percentage recoveries are 100.45 +/- 1.899 and 100.45 +/- 0.659. The results were compared with the reported spectrophotometric method. According to the variance ratio test [F test] and Student's t-test, there is no significant difference between the two methods, with respect to the precision and accuracy

Physical and chemical characteristics of crude lupinseed oil

The present work aims to study the physical and chemical characteristics of the crude lupinseed oils extracted from Giza 1, Giza 2 and Balady varieties cultivated in Egypt. The results obtained showed the following: 1. The specific gravity was 0.9240, 0.9169 and 0.9223 for crude oil extracted from Giza 1, Giza 2 and Balady respectively, while the refractive index of the same oils was as 1,471, 1,471 and 1,473, respectively. 2. The colour measured by Lovibond tintomuter in a 1.5 inch cell was 15, 14 and 9 red units and 8.5, 3.7 and 1.3 blue units for oils obtained from Giza 1, Giza 2 and Balady respectively. 3. No difference in melting point of the oil extracted from different lupinseed varieties was found, being 2C. 4. The chemical composition of oil extracted from Giza 1, Giza 2 and Balady varieties was found to be 1.86% 1.79% and 1.27%; 181.09, 171.12 and 177.46; 3.17%, 3.30% and 3.50%; 117.97, 110.87 and 130.77; 28.3°C, 28.9°C and 27.2°C; and 9.50%, 9.41% and 9.46% for free fatty acids, saponification value, unsaponifiable matter, Iodine value, titer point and the glycerol content respectively. Mean while the peroxide value of all extracted oils was zero. 5. Oleic acid was 36.24%, 47.0% and 38.49% of total fatty acids found in crude oil of Giza 1, 2 and Balady respectively, while linoleic acid and linolenic acid were 29.93 and 14.83%; 23.21 and 11.73%; 34.15 and 16.47% respectively for the same crude oil investigated. However, saturated fatty acids being palmitic acid and stearic acid represented 18.53 and 0.45; 18.02 and 0.0; 10.86 and 0.0% respectively. The total unsaturated fatty acids ranged from 10.86% to 18.98% of the total fatty acids found in crude lupinseed oils

Chromatographic analysis of Egyptian lupinseed oil

Crude lupinseed oil extracted from the varieties Giza 1, Giza 2 and Balady was classified and identified for its content of total glycerides, phospholipids, hydrocarbons, sterol ester and wax ester, free sterol and free alcohols, glycolipids and unidentified waxy materials. Classification of crude lipids by column chromatography showed that oil of GIZA 1, Giza 2 and Balady contains the following components respectively; 0.5, 0.7 and 0.8% hydrocarbons; 3.8, 3.7 and 3.5% sterol ester and wax ester; 87.14%, 86.88% and 86.58% triglycerides; 2.0% 2.3% and 1.8% phospholipids; 2.7%, 2.5% and 3.1% free sterols and free alcohols; 0.66%, 0.54% and 0.72% glycolipids. Identification of the glycerides by thin layer chromatography indicted that glycerides of oils of Giza 1, Giza 2 and Balady were 92.83, 92.89 and 92.93% triglycerides; 3.09, 2.97% and 2.95% 1,2-diglycerides; 3.38, 3.31 and 3.49% 1,3-diglycerides; 0.42, 0.53 and 0.40% 1-mono-glycerides; 0.28, 0.30 and 0.23% 2-mono -glycerides; respectively. Sitosterol, camp sterol, stigmasterol and cholesterol were detected in varied percentages in crude lupinseed oils. Site sterol represented 84.63, 85.15 and 86.51% of the total sterols found in lupinseed oil of Giza 1, Giza 2 and Balady respectively while camp sterol represented 6.86, 8.54 and 7.59% for the same varieties respectively. Meanwhile, stigma sterol and cholesterol were 6.01 and 2.50%; 4.87% and 1.44%; 4.38% and 1.52% of the total sterols found in Giza 1, Giza 2 and Balady respectively. Gas liquid chromarography analysis revealed that hydrocarbons found in crude oil of Giza 1, Giza 2 and balady was as follows: 0.90%, 0.41% and 0.69% C[17]; 0.75%, 0.91% and 0.41% C[18]; 1.13,% 0.91% and 0.55% C[19]; 74.05%, 84.66% and 77.26% C[23]; 2.11%, 1.28% and 0.25% C[24]; 3.93%, 3.20% and 1.93% C[25]; 7.05%. 2.97% and 8.69% C[27]; 10.07%, 5.49% and 10.21% C[31] respectively

Technological aspects of Egyptian lupinseed oil

Crude oils obtained from Lupine seed of Giza 1, Giza 2 and Balady were treated by neutralization and bleaching. Fuller's earths, mixture of Fuller's earth and charcoal as well as bleaching by heat alone were used in the bleaching process. The obtained results revealed the following: 1.The effect of neutralization on colour was more pronounced. Blue pigments were removed completely, while the red units of crude lupine seed oil of Giza 1, Giza 2 and Balady were 15, 14 and 9 respectively. The red colour of all samples was reduced by neutralization as it reached 13.1, 7.5 and 8.5 respectively. However, melting point of all samples remained stable. 2. Free fatty acids of crude oil of Giza 1, Giza 2 and Balady decreased after neutralization. Meanwhile, the peroxide value of all crude lupine seed oils increased. 3. Unsaponifiable matter and titer point decreased slightly by neutralization of crude lupine seed oils. Besides the iodine value of crude oil of Giza 1, Giza 2 and Balady was found to decrease from 117.97, 110.87 and 130.77 to 113.56, 107.53 and 126.22 respectively for the same neutralized oils. 4. Bleaching of neutralized oil of Giza 1, Giza 2 and Balady lupine by 2% Fuller's earth caused an increase in the free fatty acids content. The increase was more pronounced in lupinseed oil of Giza 1. The free fatty acids were 0.08, 0.08 and 0.09% for neutralized oil of Giza 1, Giza 2, and Balady respectively. After bleaching they became 0.15, 0.10 and 0.10% respectively. 5. A mixture containing 95% Fuller's earth and 5% charcoal in an amount of 3% was more active in bleaching than using 2% of Fuller's earth alone. 6. Heat bleaching method was found to be more effective in removing red colour units from lupine seed oils compared with 3% mixture of fullers earth and charcoal. The colour of oils obtained from Giza 1, Giza 2 and balady bleacher by 3% huller's earth and charcoal were as 8.0, 4.5 and 5.6 Lovibond red units respectively, while were 6.7, 4.1 and 5 when bleaching was carried out by heat bleaching method