Selectivity as one of the crucial validation parameters was extensively evaluated during the forced degradation study and validation. A final consideration is the inherent variation within a particular vitamin assay and laboratory Table 23. Bjerrum developed the first general method for the determination of stability constants of metal-ammine complexes in 1941. Examples would include high magnesium products high pH , intake-limiting products such as acidified liquid feeds, and dry products containing high levels of urea or other strongly hygroscopic ingredients. Vitamins D 2 and D 3 are about equal in activity in all mammals. A chromatogram of the vitamin D 3 sample after thermal degradation in water: a fragment of vitamin D 3 and b—d hydroxy vitamin D 3.
All samples were exposed to selected stress conditions for 24 h at 25 and 60°C. Method precision and accuracy were examined in terms of repeatability, intermediate precision and accuracy intra- and inter-day during three validation days, based on three different quality control samples covering the whole analytical range. According to the results of forced degradation study, vitamin D 3 was found to be the most prone to degradation under acidic and oxidizing conditions. The validated method was further applied to assay the content of vitamin D 3 in commercially available pharmaceuticals. Injection repeatability was evaluated on three concentration levels by re-injecting the same quality control sample six times. Vitamin D 3 eluting at a retention time of 2. A general comparison of the spray-dried and beadlet product form is shown in Table 21.
Vitamins are a group of chemically diverse compounds that vary considerably in their stability and susceptibility to destruction by physical and chemical agents. Ergocalciferol decomposed rapidly at 25 and 40° when stored in dry air. The proposed method enables direct determination of vitamin D 3 in various liquid pharmaceutical preparations and nutritional supplements without any pretreatment. The limitations of extemporaneous manufacture support the use of commercial products when possible. Stress samples after thermal and alkaline degradation show comparable chromatograms Figure B , with a single peak for vitamin D 3. Solid dosage forms Three batches of commercially available nutritional supplements from two different producers preparations E and F prepared in triplicate were analyzed.
The formulations passed microbial testing after 9 months. The rankings may vary depending on product form and conditions of manufacturing and storage; however, the overall relationship among vitamins is consistent with previous studies Frye, 1994. Introduction Vitamin D 3 cholecalciferol is a unique fat-soluble vitamin because it can be obtained by endogenous synthesis. Product Forms Strategies for improving vitamin stability through product formulation have been developed since the beginning of commercial vitamin synthesis in the 1950s, using specific criteria Table 20. To broaden the analytical range of the method, calibration standards were reanalyzed with variations of the injection volume Table. The quality control samples were kept in the autosampler at 25°C and analyzed at 0, 6, 24 and 48 h. Because feed products are complex and multiple interactions can occur between formulation, manufacturing, storage conditions and time, feed manufacturers should ideally develop their own databases of vitamin activities.
Low vitamin D 3 concentrations in nutrition supplements and prescription medicines, the presence of excipients that might interfere with its determination and its lipophilic nature can lead to various analytical problems in the identification and quantification of the vitamin. Activated vitamin D receptors in intestine and bone maintain calcium absorbance and homeostasis. Its levels vary during the menstrual cycle. The stability of individual vitamins in premixes and finished feeds varies according to a number of factors. Factors Affecting Vitamin Stability A number of common physical and chemical factors affect the stability of vitamins in premixes and finished feeds Figure 4 Gadient, 1986; Frye, 1994; Reddy and Love, 1999. The rate of acid hydrolysis was very rapid and resulted in complete degradation of vitamin D 3 within 1 h. For the current unit quantity, please visit the.
This technique is especially convenient for quantification of the vitamin D 3 in various complex matrixes and multivitamin mixtures —. Method application: assay of vitamin D 3 in commercial nutrition supplements and prescription medicines The validated method was applied to assay the content of vitamin D 3 in commercial liquid prescription medicines A, B and C, liquid nutrition supplement D and solid nutrition supplements E and F. Recoveries were calculated using the same formula as for liquid preparations. Likewise, a defined number of samples of finished products can be obtained from warehouses and retail locations during the year for vitamin analysis. Cholecalciferol contents were assayed using ultra-performance liquid chromatography.
It is chemically similar to cholesterol which is obtained from animals. The vitamin manufacturing industry has developed products of high purity and quality, with improved stability, high bioavailability and optimum handling and mixing properties. The injection volume was set between 3 and 50 µL, depending on the type of the preparation. Appropriate volumes of the working standard solution were pipetted into separate amber vials, diluted to a volume of 1,000 µL with methanol and mixed, resulting in the following concentrations: 0. The injection volume was 50 µL.
Ergocalciferol decomposed rapidly at 25 and 40° when stored in dry air. It is converted to ergocalciferol vitamin D 2 upon irradiation by ultraviolet light or electronic bombardment. Great difficulties may be surmounted by patience and perseverance. Choice of laboratory and use of adequate sampling and assay replication can overcome this problem. Decomposition of ergocalciferol led to the formation of products of higher polarity.
In addition, liquid and solid nutritional supplements and prescription medicines were analyzed to confirm the adequacy of the method. The method was also found selective in the presence of the formed degradation products during the forced degradation study. D 3 Pre-vitamin D 3 2. Background: Vitamin D deficiency states in children are treated with extemporaneously prepared oral cholecalciferol liquid in olive oil at The Children's Hospital at Westmead. Packaging Unit quantity: 500 mg. It is oxidized and inactivated by moist air within a few days.
For further information and support please go to the website of the. The calibration plot for the drug was linear in the range 0. Bjerrum went on to determine the stability constants for systems in which many complexes may be formed. Severe vitamin D deficiency manifests as rickets in infants and children, and osteomalacia in the elderly. Additional confirmation that these degradation products are vitamin D 3 isomers was performed by product ion scan mode, which showed the same fragmentation profiles Table.