Analysis of Fat-Soluble Vitamins. XX. Determination of Vitamin D in Multivitamin Preparations. Second Collaborative Study

1978 ◽  
Vol 61 (3) ◽  
pp. 731-734
Author(s):  
Ellen J De Vries ◽  
Frits J Mulder ◽  
Ben Borsje
Keyword(s):  
Vitamin D ◽  
Vitamin A ◽  
Test Data ◽  
Vitamin D3 ◽  
Collaborative Study ◽  
Three Samples ◽  
The Mean ◽  
Fat Soluble Vitamins

Abstract The official first action method for determining vitamin D in multivitamin preparations was modified. The method was collaboratively studied by 7 laboratories, using 6 preparations in oil. The preparations consisted of vitamin D at various levels and at various ratios (in w/w) to vitamin A. Three samples contained cholecalciferol and 3 samples contained vitamin D3 from vitamin D3 resin. After outliers were eliminated by the Dixon test, data were analyzed and averages were compared with amounts of vitamin D known to be in each sample. For samples with vitamin D: vitamin A ratios of 1:0.5, 1:5, and 1:10, the mean vitamin D recoveries were 98.8, 94.6, and 90.7%, respectively. The method has been adopted as official final action.

Analysis of Fat-Soluble Vitamins. XX. Determination of Vitamin D in Multivitamin Preparations. Second Collaborative Study

1978 ◽  
Vol 61 (3) ◽  
pp. 735-745
Author(s):  
Ellen J De Vries ◽  
Frits J Mulder ◽  
Ben Borsje
Keyword(s):  
Vitamin D ◽  
Vitamin A ◽  
Test Data ◽  
Vitamin D3 ◽  
Collaborative Study ◽  
Three Samples ◽  
The Mean ◽  
Fat Soluble Vitamins

Abstract The official first action method for determining vitamin D in multivitamin preparations was modified. The method was collaboratively studied by 7 laboratories, using 6 preparations in oil. The preparations consisted of vitamin D at various levels and at various ratios (in w/w) to vitamin A. Three samples contained cholecalciferol and 3 samples contained vitamin D3 from vitamin D3 resin. After outliers were eliminated by the Dixon test, data were analyzed and averages were compared with amounts of vitamin D known to be in each sample. For samples with vitamin D: vitamin A ratios of 1:0.5, 1:5, and 1:10, the mean vitamin D recoveries were 98.8, 94.6, and 90.7%, respectively. The method has been adopted as official final action.

Analyses of Fat-Soluble Vitamins, XIV. Collaborative Study of the Determination of Vitamin D in Multivitamin Preparations

1977 ◽  
Vol 60 (1) ◽  
pp. 151-154
Author(s):  
Frits J Mulder ◽  
Ellen J De Vries ◽  
Ben Borsje
Keyword(s):  
Vitamin D ◽  
Polyethylene Glycol ◽  
Vitamin A ◽  
Colorimetric Assay ◽  
Collaborative Study ◽  
Official Method ◽  
Colorimetric Determination ◽  
Trans Isomers ◽  
Decomposition Products

Abstract The colorimetric assay for the determination of vitamin D (4000—50,000 international units (IU)/g) in multivitamin preparations has been collaboratively studied. The method is based on the same principle as the official method for the determination of vitamin D in concentrates, i.e., elimination of trans-isomers of vitamin D resins. The method includes the following steps: saponification and extraction (isolation of unsaponifiable material), phosphate-treated alumina column chromatography (elimination of tocopherols and vitamin A decomposition products), partition chromatography with polyethylene glycol 600 and Celite (separation of vitamin D fraction from vitamin A alcohol), adsorption chromatography on Florex (elimination of vitamin A decomposition products and small amounts of polyethylene glycol 600), maleic anhydride addition reaction (elimination of trans-isomers of vitamin D resins), and colorimetric determination at 2 wavelengths with and without acetic anhydride (an inhibitor for the color reaction of vitamin D and antimony trichloride). The mean result of 4 laboratories for 8 different samples, expressed as per cent of the known amount of vitamin D added, was 95.8% with a coefficient of variation of 10.5%. Considering the complexity of the method, the collaborative results were reasonable. The method has been adopted as official first action.

Factors Influencing the Vitamin A and D Potency of Grayfish Liver Oil Squalus sucklii (Girard)

1939 ◽  
Vol 4b (5) ◽  
pp. 312-322 ◽  
Author(s):  
L. I. Pugsley
Keyword(s):  
Vitamin D ◽  
Vitamin A ◽  
Significant Influence ◽  
The Other ◽  
Factors Influencing ◽  
Three Samples ◽  
The Mean ◽  
Yield Colour

A study of the variations in yield, colour and vitamin A potency of the liver oil of grayfish, Squalus sucklii (Girard), as influenced by sex, size and time of catching was made. The mean yield (71.5 per cent), colour (3.5 Lovibond units of yellow) and vitamin A potency (3330 blue units per g.) varied with size of the fish; the other factors did not show any significant influence. Three samples of liver oil assayed 4, 6 and 7 international units of vitamin D and the values did not show any relation to the vitamin A potency.

Analysis of Fat-Soluble Vitamins. XXIX. Liquid Chromatographic Determination of Vitamin D in AD Concentrates: Collaborative Study

1985 ◽  
Vol 68 (5) ◽  
pp. 822-825
Author(s):  
Ellen J De Vries ◽  
Ben Borsje
Keyword(s):  
Vitamin D ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Single Column ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
High Level ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract A simplified liquid chromatographic (LC) method for determining vitamin D in vitamin AD concentrates (> 5000 IU vitamin D/g) was collaboratively studied. In the simplified method, the 2 columns specified in AOAC LC method 43.101-43.109 are replaced by a single column, which separates the vitamin D isomers and the vitamin A esters. The procedure for oils includes dissolution and quantitation by normal phase LC. Dry multivitamin concentrates and aqueous dispersions are treated with an enzyme system and the vitamins are extracted with n-pentane. Six coded samples were distributed to 16 laboratories; 15 collaborators returned their results. Estimates of repeatability and reproducibility for the oil samples were 1.1 and 3.1%, respectively; for the high-level concentrated dry preparation 1.4 and 3.9% and for the low-level concentrated dry preparation 1.3 and 11.4%, respectively. These values are a considerable improvement over the results obtained in the 1979 multivitamin collaborative study. The method has been adopted official first action for determination of vitamin D in vitamin AD concentrates containing s 5000 IU vitamin D/g.

Retinol, α-Tocopherol and Vitamin D3 in White MuscleDisease

2018 ◽  
Vol 74 (1) ◽  
pp. 6029-2018
Author(s):  
HANDAN MERT ◽  
SERKAN YİLDİRİM ◽  
IBRAHİM HAKKİ YORUK ◽  
KİVANC IRAK ◽  
BAHAT COMBA ◽  
...  
Keyword(s):  
Vitamin A ◽  
Vitamin D3 ◽  
White Muscle ◽  
Bone Structure ◽  
Early Stage ◽  
Vitamin A Deficiency ◽  
Muscle Disease ◽  
Control Group ◽  
White Muscle Disease ◽  
Fat Soluble Vitamins

Vitamins are essential for the health of all living organisms. Vitamins E, A, D and K are known as fat-soluble vitamins, and deprivation of vitamin E causes various disorders, especially in the reproduction and cardiovascular systems and in muscle functions. Vitamin A, on the other hand, has roles in various biological functions – like eyesight – and the growth, reproduction and differentiation of epithelial cells. Vitamin A deficiency leads to the keratinization of the epithelium, and disorders related to the metaplasies of the genital and genitourinary systems. Conversely, vitamin D is defined as a pro-hormone and is responsible for Cahomeostasis, and thus indirectly affects the bone metabolism, bone structure, and cellular and neural functions of Ca. White muscle disease (WMD) can occur in newborn lambs, but is more commonly seen in lambs of up to 3 months of age. In this study, 30 lambs of 3 to 50-days-old from different flocks diagnosed with White Muscle Disease (WMD) were selected as research material, while the control group consisted of 8 healthy lambs. With the aim of clarifying the cause of WMD, serum fat-soluble vitamins, retinol, α-tocopherol and vitamin D3 levels were determined in 16 lambs. Gluteal and heart musclet issue samples also were taken from 30 lambs with WMD. The vitamin levels of the samples were analysed by HPLC. The levels of serum α-tocopherol, retinols, and vitamin D3 were foundto be low in the diseased animals, but only retinol (p<0.001) and α-tocopherol (p<0.0011) level differences were statistically relevant. Macroscopically, Zenker’s necrosis was determined in the heart muscles of 17 lambs, and in the gluteal and chest muscles of 6 lambs. 7 lambs displayed necrosis in both their heart and in gluteal muscles. The samples were analyzed microscopically to reach similar findings: swollen homogeneous pink muscles, pycnotic nuclei, and hyperaemic and haemorrhagic blood vessels in gluteal, chest and heart muscles. Hyaline degeneration and Zenker's necrosis, dystrophic regions in necrotic areas, cc was detected as a severe disease in lambs at an early stage of life with advanced degeneration in different muscle tissues. Deficiency of fat-soluble vitamins was also detected in the sick animals. Control group lambs had higher levels of α tocopherol and retinol (p<0.001) compared to the sick lambs. .

scholarly journals Oral Vitamin D3 Supplementation for Femtosecond LASIK–Associated Dry Eye

2021 ◽  
Author(s):  
Ying Lin ◽  
Huanjun Su ◽  
Jianbin Wu ◽  
Muzhi Yuan ◽  
Yong Zhang
Keyword(s):  
Vitamin D ◽  
Dry Eye ◽  
Vitamin D3 ◽  
Serum Vitamin ◽  
Control Group ◽  
Oral Vitamin ◽  
Serum Vitamin D ◽  
The Mean ◽  
Experimental Group ◽  
Schirmer I Test

Abstract Purpose: To assess the effect of oral vitamin D3 supplementation in dry eye after femtosecond laser-assisted in situ keratomileusis (FS-LASIK).Setting: Liuzhou Worker’s Hospital.Design: This prospective study included 90 patients selected between January and December in 2019, who underwent fs-lasik operation in our hospital and had obvious symptoms indicating dry eyes one month after operation. The subjects were randomly divided into two groups: the experimental group (n = 45) received vitamin D3 2000 IU / D continuously for 12 weeks; the control group (n = 45) did not take vitamin D3 orally. Ocular surface disease index（OSDI）, tear breakup time（TBUT）and Schirmer’s Test I were evaluated pre-medication and 1,3,6 months after treatment. Serum vitamin D level, and the mean concentration of cytokine IL-6, IL-17, IL-23 in tears were also measured. Results: One month after treatment, the mean OSDI score of the experimental group (11.67 ± 8.53) was significantly lower than that of the control group (23.82 ± 13.22) (P = 0.007). TBUT (10.71±1.02s) and Schirmer I (9.36±0.40mm) of the experimental group were higher than those of the control group (7.49±1.29 s and 7.51±0.44 mm). The OSDI (10.25 ± 5.49), TBUT (10.75±1.09 seconds) and Schirmer I test value (11.34±0.39 mm) of the experimental group were significantly lower than those of the control group (20.22±6.23, 8.36±1.23， 8.12±0.50) at 3 months after treatment. There were significant differences in OSDI, TBUT (P ＜ 0.05) and Schirmer I test value between the two groups at 6 months after treatment. Serum vitamin D3 level was negatively correlated with OSDI score (r=-0.90；P=0.00), and positively correlated with Schirmer I test (r=0.88；P=0.00), TBUT score (r=0.89；P=0.00) and TMH (r=0.80；P=0.00). IL-17 level was shown to be significantly correlated with TBUT (r=-0.25, P=0.014) and Schirmer I test (r=-0.21, P=0.018). IL-6 level was significantly correlated with OSDI (R=0.18, P = 0.020) and TBUT (R=0.20, P = 0.019).

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.

Determination of Maleic Hydrazide Residues in Tobacco and Vegetables

1973 ◽  
Vol 56 (5) ◽  
pp. 1164-1172
Author(s):  
Milan Ihnat ◽  
Robert J Westerby ◽  
Israel Hoffman
Keyword(s):  
Standard Deviation ◽  
Present Method ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Official Method ◽  
Sample Weight ◽  
Relative Standard ◽  
The Mean ◽  
Pipe Tobacco

Abstract The distillation-spectrophotometric method of Hoffman for determining maleic hydrazide has been modified to include a double distillation and was applied to the determination of 1–30 ppm maleic hydrazide residues in tobacco and vegetables. Recoveries of 1–23 μg added maleic hydrazide were independent of weight of maleic hydrazide, but did depend on sample and sample weight. The following recoveries were obtained from 0.5 g sample: pipe tobacco, 84%; commercially dehydrated potato, 83%; cigar tobacco, 81%; dried potato, 76%; fluecured tobacco, 73%; dried carrot, 71%. In the absence of sample, the recovery was 82%. When appropriate standard curves were used, maleic hydrazide levels determined in tobacco samples were essentially independent of sample weight in the range 0.1–3 g. The mean relative standard deviation for a variety of field-treated and fortified tobacco samples containing 1–28 ppm maleic hydrazide was 3%. The precision and sensitivity of this procedure seem to be substantial improvements over official method 29.111–29.117. It is recommended that the present method be subjected to a collaborative study.

Liquid Chromatographic Determination of Diazepam in Tablets: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was &lt; 1.5%. The method has been adopted official first action.

scholarly journals Determination of Cholecalciferol (Vitamin D3) in Selected Foods by Liquid Chromatography: NMKL Collaborative Study

2003 ◽  
Vol 86 (2) ◽  
pp. 400-406 ◽  
Author(s):  
Anders Staffas ◽  
Arne Nyman ◽  
K Ask ◽  
E Hermansson ◽  
J S Jacobsen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Fish Oil ◽  
Vitamin D3 ◽  
Collaborative Study ◽  
The Other ◽  
Vitamin D2 ◽  
Cooking Oil ◽  
Relative Standard

Abstract Results are presented from an NMKL (Nordic Committee on Food Analysis) collaborative study of a method for the determination of cholecalciferol (vitamin D3) in foods. The method is based on the addition of an internal standard (vitamin D2), followed by saponification and extraction with n-heptane. The fraction that contains vitamin D2/D3 is separated by preparative normal-phase liquid chromatography (LC), and the analytes are determined by reversed-phase LC with UV detection at 265 nm. The method was tested by 8 participating laboratories. In this study 6 different matrixes were analyzed for cholecalciferol content: milk, liquid infant formula (gruel), cooking oil, margarine, infant formula, and fish oil. The contents varied from 0.4 to 12 μg/100 g. Three matrixes (milk, gruel, and margarine) were fortified with vitamin D3. In the other matrixes, vitamin D3 was added at 3 different levels at the Swedish National Food Administration. The milk was analyzed as a blind duplicate, whereas the other matrixes were analyzed as split-level pairs. The recoveries from the samples with vitamin D3 added varied from 93 to 102%. The repeatability relative standard deviation (RSDr) values for accepted results varied between 2.2% (fish oil) and 7.4% (cooking oil), whereas the reproducibility relative standard deviation (RSDR) values varied between 6.8% (margarine) and 24% (cooking oil).

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