Analysis of Fat-Soluble Vitamins. XXIII. High Performance Liquid Chromatographic Assay for Vitamin D in Vitamin D3 and Multivitamin Preparations1

1979 ◽  
Vol 62 (6) ◽  
pp. 1285-1291
Author(s):  
Ellen J De Vries ◽  
Jakob Zeeman ◽  
Robert J E Esser ◽  
Ben Borsje ◽  
Frits J Mulder
Keyword(s):  
Vitamin D ◽  
Vitamin D3 ◽  
Coefficient Of Variation ◽  
High Performance ◽  
Conversion Factor ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
External Standard ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract Vitamin D is determined in preparations containing other fat-soluble vitamins by high performance liquid chromatography (HPLC). The unsaponifiable residue is extracted and separated from interferences by reverse phase chromatography; the fraction corresponding to vitamin D3 is collected and quantitated using normal phase chromatography (amylalcohol-n-hexane as mobile phase) by measuring the vitamin D3 and previtamin D3 peaks at 254 nm. Previtamin D3 content is calculated as vitamin D3 with a conversion factor (determined on the equipment used). Application of the method to vitamin AD3 mixtures in oils gives 98-102% recovery. The reproducibility, using an external standard, is 2-3%, calculated as the coefficient of variation; with an internal standard, the coefficient of variation is 1-1.5%. The method measures potential vitamin D3 content in preparations containing ≽ 200 IU/g in the presence of all known vitamin D3 isomers, vitamin A, and vitamin E.

Analysis of Fat-Soluble Vitamins. XXVI. High Performance Liquid Chromatographic Determination of Vitamin D in Fortified Milk and Milkpowder

1982 ◽  
Vol 65 (5) ◽  
pp. 1225-1227
Author(s):  
Ben Borsje ◽  
Ellen J De Vries ◽  
Jakob Zeeman ◽  
Frits J Mulder
Keyword(s):  
Vitamin D ◽  
Vitamin D3 ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Fortified Milk ◽  
Liquid Chromatographic Determination ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract Vitamin D is determined by high performance liquid chromatography (HPLC) in samples containing other fat-soluble vitamins. The vitamin D in the unsaponifiable residue is extracted and separated from interferences by straight phase chromatography, and the fraction corresponding to vitamin D3 is collected and quantitated using the AOAC official final action HPLC method for vitamin D3. Analysis of a synthetic mixture gave reasonable recoveries. The method measures potential vitamin D3 content in milkpowder samples containing 2IU vitamin D/g in the presence of all known vitamin D3 isomers, vitamin A, and vitamin E.

Analysis of Fat-Soluble Vitamins. XXIV. High Performance Liquid Chromatographic Determination of Vitamin D in Vitamin D Resin Containing Powders: Collaborative Study1

1981 ◽  
Vol 64 (1) ◽  
pp. 58-60
Author(s):  
Frits J Mulder ◽  
Ellen J De Vries ◽  
Ben Borsje ◽  
◽  
L Ameika ◽  
...  
Keyword(s):  
Vitamin D ◽  
Vitamin D3 ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Dry Powders ◽  
Liquid Chromatographic Determination ◽  
The Difference ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract Further study of vitamin D methodology solved the discrepancy between the AOAC chemical method, 43.068-43.078, and the HPLC assay for vitamin D3 in resin containing dry powders. The discrepancy is caused by the difference in solubility of the vitamin D3 resin in benzene and in pentane. The method has been modified accordingly, and has been adopted official first action for vitamin D3 resins and vitamin D3 resin containing powders and aqueous dispersions.

Analysis of Fat-Soluble Vitamins. XXII. High Performance Liquid Chromatographic Determination of Vitamin D in Concentrates. Collaborative Study1

1979 ◽  
Vol 62 (5) ◽  
pp. 1031-1040
Author(s):  
Frits J Mulder ◽  
Ellen J De Vries ◽  
Ben Borsje
Keyword(s):  
Vitamin D ◽  
High Performance ◽  
Chemical Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
De Vries ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract A collaborative study was carried out which compared the official chemical method (43.B14- 43.B24), the HPLC method according to Hofsass et al. including maleic anhydride treatment, and the HLPC procedure according to De Vries et al. for vitamin D concentrates. A total of 396 samples were distributed to 33 collaborators for analysis. Five laboratories performed both the chemical and the HPLC methods. Five laboratories performed the Hofsass method and 16 laboratories performed the De Vries method. The results for the chemical method agreed with the theoretical values for the samples, and the standard deviation was comparable to that obtained in previous AOAC collaborative studies. Collaborative results for the Hofsass method were low. In addition, incorrect use of a fixed conversion factor (1/0.586) and necessity of a double chromatographic system on a non-treated and a treated vitamin D sample reduce the effectiveness of the method. There were no adverse reactions to the De Vries HPLC method. It is recommended that the method be adopted official first action as an alternative procedure for determining vitamin D in concentrates, excluding powders containing irradiated 7-dehydrocholesterol.

Liquid-chromatographic measurement of creatinine in serum and urine.

1983 ◽  
Vol 29 (5) ◽  
pp. 851-853 ◽  
Author(s):  
T Okuda ◽  
T Oie ◽  
M Nishida
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
External Standard ◽  
Chromatographic Measurement ◽  
Liquid Chromatographic ◽  
Serum And Urine

Abstract We describe the adaptation of a "high-performance" liquid chromatographic method for determination of creatinine in serum and urine. The proposed method is simple, rapid, precise, and accurate. The retention time for creatinine can be varied simply by changing the KH2PO4 concentration in the mobile phase: acetonitrile/aqueous KH2PO4 (1/4 by vol). Within-day precision (CV) was 1.2-3.6% in serum chromatographed with an internal standard, and 2.3-2.8% in serum when an external standard was used. Between-day precision (CV) was 1.3-2.1% in serum and 1.3-2.7% in urine (with an external standard). Analytical recoveries of creatinine added to serum were 94-100% for the method with an internal standard, 95-103% with an external standard.

Analysis of Fat-Soluble Vitamins. XXV. High Performance Liquid Chromatographic Determination of Vitamin D in Multivitamin Preparations: Collaborative Study1

1981 ◽  
Vol 64 (1) ◽  
pp. 61-70
Author(s):  
Ellen J De Vries ◽  
Frits J Mulder ◽  
Ben Borsje ◽  
◽  
L Ameika ◽  
...  
Keyword(s):  
Vitamin D ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Phase System ◽  
Single Column ◽  
Liquid Chromatographic Determination ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract The HPLC method for determining vitamin D in multivitamin preparations was studied collaboratively. Samples were distributed to 43 laboratories in 10 countries. Twenty-four laboratories gave their results. The method specifies a reverse phase system for the cleanup and a straight phase system for the determination. Difficulties arise when laboratories are equipped with HPLC apparatus with a single column. Laboratories experienced in vitamin D analysis reported good results, even if they were equipped with a single column HPLC apparatus. Eleven of the 24 laboratories reported satisfactory results. For this rather complicated method, the coefficient of variation for a single assay is acceptable. The method has been adopted official first action as an alternative procedure to the chemical method for determining vitamin D in multivitamins.

Analysis of Fat-Soluble Vitamins. XXVII. High Performance Liquid Chromatographic arid Gas-Liquid Chromatographic Determination of Vitamin D in Fortified Milk and Milkpowder: Collaborative Study

1982 ◽  
Vol 65 (5) ◽  
pp. 1228-1234
Author(s):  
Ellen J De Vries ◽  
Ben Borsje ◽  
◽  
L Ameika ◽  
N T Baillies ◽  
...  
Keyword(s):  
Vitamin D ◽  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Fortified Milk ◽  
Whole Milk ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract A collaborative study of the high performance liquid chromatographic (HPLC) method for vitamin D in fortified milkpowder (skimmed and whole milk) and a milkpowder preparation was carried out on 182 samples distributed to 26 laboratories. Thirteen laboratories submitted results. The level of vitamin D was 2-7IU vitamin D3/g milkpowder. All samples also contained vitamin A. Three laboratories were excluded from the statistical evaluation because of incomplete results or deviation from the analytical procedure. Other laboratories reported acceptable results. At the same time, 63 samples were distributed to 9 laboratories which used a gas-liquid chromatographic method for determining vitamin D in milkpowder. Only one laboratory reported results. The HPLC method has been adopted official first action.

Analysis of Fat-Soluble Vitamins. XVIII. Interlaboratory Comparison of Vitamin D Assay Methods

1978 ◽  
Vol 61 (1) ◽  
pp. 122-128
Author(s):  
Ben Borsje ◽  
Heinz A H Craenen ◽  
Robert J E Esser ◽  
Frits J Mulder ◽  
Ellen J Vries
Keyword(s):  
Vitamin D3 ◽  
High Performance ◽  
Interlaboratory Comparison ◽  
High Performance Liquid Chromatographic ◽  
The Third ◽  
Confirmation Test ◽  
Aoac Method ◽  
Assay Methods ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract Nine laboratories determined the vitamin D3 content of 4 samples in oil containing, in addition to vitamin D3, different amounts of tachysterol3, isotachysterol3, trans-vitamin D3, lumisterol3, and 7-dehydrocholesterol, in order to assess the effect of these isomers on the assay. The analyst selected the method to be used. Three high performance liquid chromatographic (HPLC) methods were applied: 2 were direct and the third required prior isolation of the unsaponifiable material. The 6 remaining analysts used gas-liquid chromatographic (CLC) methods; all GLC techniques required saponification and silylation, and 3 required an additional pretreatment. The results from the GLC and HPLC methods were compared with the known composition of the samples and the results obtained by the official AOAC method, 43.B14–43.B24. The samples were also analyzed by the AOAC method without the maleic anhydride reaction and by the AOAC method with correction for the isotachysterol content. The results of the HPLC assays showed that this technique is promising, but improvements are still needed. The precision and accuracy of the GLC assays varied. However, satisfactory results were obtained after extensive prepurifications. The AOAC chemical method was satisfactory for those samples shown suitable by the confirmation test, i.e., in the absence of isotachysterol.

scholarly journals A Simple and Sensitive HPLC Method for Simultaneous Analysis of Nabumetone and Paracetamol in Pharmaceutical Formulations

2011 ◽  
Vol 8 (s1) ◽  
pp. S41-S46
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Dillipkumar Sahoo
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Aqueous Acetic Acid ◽  
Linear Calibration ◽  
Acceptance Range ◽  
Liquid Chromatographic

This paper describes a high-performance liquid chromatographic method for simultaneous estimation of nabumetone and paracetamol in binary mixture. The method was based on RP-HPLC separation and quantitation of the two drugs on hypersil C-18 column (250 mm × 4.6 mm) using a mobile phase consisting of acetonitrile and 0.05% aqueous acetic acid (70:30v/v) at flow rate of 1 mL min-1. Quantitation was achieved with PDA detector at 238 nm based on peak area with linear calibration curves at concentration ranges 5-25 µg mL-1for both the drugs. Naproxen sodium was used as internal standard. The method has been successively applied to pharmaceutical formulation. No chromatographic interference from the tablet excipients was found. The method was validated in terms of precision, robustness, recovery and limits of detection and quantitation. The intra and inter-day precision and accuracy values were in the acceptance range as per ICH guidelines.

scholarly journals Determination of Finasteride in Tablets by High Performance Liquid Chromatography

2007 ◽  
Vol 4 (1) ◽  
pp. 109-116 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Official Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug ◽  
Liquid Chromatographic

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

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