Rapid determination of vitamin D3 in milk-based infant formulas by liquid chromatography-tandem mass spectrometry

Kwak, Byung‐Man; Jeong, In-Seek; Lee, Moon-Seok; Ahn, Jang‐Hyuk; Park, Jong‐Su

doi:10.1016/j.foodchem.2014.05.137

Cited by 20 publications

(14 citation statements)

References 14 publications

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“…A recently reported method on fat soluble vitamins and carotenoids in selected plant foods quantified four carotenoids and six fat soluble vitamins within 30 min and with good intra-day precision ranged between 3 and 7% (Gentili & Caretti, 2011). Several methods have been addressed on quantification of vitamin D 3 (Kwak, Jeong, Lee, Ahn, & Park, 2014) and vitamin A (Lim, Kim, Ahn, & Kim, 2011) in infant formula in recent literature with good repeatability, but with longer run times of 70 min and 30 min respectively. Twelve target analytes in milk from different species were quantified in another method, but in two separate columns as carotenoids in C 30 in 30 min and other fat soluble vitamins in C 18 in 22 min with intra-day precision ranged from 5-10% (Gentili et al, 2012).…”

Section: Analysis Of Multivitamin Dietary Supplements and Infant Formmentioning

confidence: 99%

Quantification of selected fat soluble vitamins and carotenoids in infant formula and dietary supplements using fast liquid chromatography coupled with tandem mass spectrometry

Nimalaratne

Sun

et al. 2014

Food Research International

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Section: Analysis Of Multivitamin Dietary Supplements and Infant Formmentioning

confidence: 99%

Quantification of selected fat soluble vitamins and carotenoids in infant formula and dietary supplements using fast liquid chromatography coupled with tandem mass spectrometry

Nimalaratne

Sun

et al. 2014

Food Research International

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“…Sample preparation process plays an important role in enhancing sensitivity and reducing matrix interference. The most common preparation technique is saponification [8,9], liquid-liquid extraction (LLE) [10], solid-phase extraction (SPE) [11][12][13][14] and derivatization [15]. Saponification is commonly the first step before LLE and SPE and is used to remove neutral lipids, especially triglycerides.…”

Section: Introductionmentioning

confidence: 99%

“…Saponification is commonly the first step before LLE and SPE and is used to remove neutral lipids, especially triglycerides. This method has been used for the determination of vitamin D in various types of food samples such as infant products [12,16], milk, cream and butter [17], human foods, pet foods and supplements [18], fish oil [19], beef and poultry [20], fortified orange juice [21], dietary supplements and vitamin premixes [22], bovine milk [11], vegetables [23], meat [24] and human serum [6]. Saponification using methanolic or ethanolic KOH at elevated temperatures (60-100°C) for 20-45 min was able to suppress lipids and proteins interferences [25].…”

Section: Introductionmentioning

confidence: 99%

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

et al. 2019

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In this study, salting-out assisted liquid–liquid extraction (SALLE) as a simple and efficient extraction technique followed by high-performance liquid chromatography (HPLC) was employed for the determination of vitamin D3 in milk samples. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. Under the optimum conditions, acetonitrile and ammonium sulfate were used as the extraction solvent and salting-out agent, respectively. The vitamin D3 extract was separated using Hypersil ODS (250x i.d 4.6 mm, 5 µm) HPLC column that was coupled with diode array detector. Vitamin D2 was used as internal standard (IS) to offset any variations in chromatographic conditions. The vitamin D3 and the IS were eluted in 18 min. Good linearity ( r 2 > 0.99) was obtained within the range of 25–600 ng g −1 with the limit of detection of 15 ng g −1 and limit of quantification of 25 ng g −1 . The validated method was applied for the determination of vitamin D3 in milk samples. The recoveries for spiked samples were from 94.4 to 113.5%.

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“…An alternative method was applied that involves initial saponification of triglycerides and other fats with strong base, followed by neutralization and liquid-liquid extraction. 43 Figure S-29 shows that saponification returns the same array of peaks as seen in extracted unsaponified supplemented feeds.…”

Section: Resultsmentioning

confidence: 81%

Vitamin D analyses in veterinary feeds by gas chromatography-tandem mass spectrometry

Lehner

Johnson

Zimmerman

et al. 2021

Eur J Mass Spectrom (Chichester)

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This report examines the feasibility of determination of Vitamin D3, D2 and their 25-hydroxy metabolites utilizing Gas Chromatography Tandem Mass Spectrometry (GC/MS/MS) as a potential alternative to popular Liquid Chromatography Tandem Mass Spectrometric (LC/MS/MS) methodologies. The GC/MS/MS approach was found to operate reasonably well despite long-standing concerns that gas-liquid chromatography of vitamin D compounds invoke thermal rearrangements owing to the relatively high inlet and capillary column temperatures used. The workup procedure involved incubation of feed samples with concentrated potassium hydroxide for overnight fat saponification, extraction of D Vitamins in n-hexane and reaction with N,O-bis(trimethylsilyl)trifluoroacetamide at 70 °C for 30 mins. In addition to parent compounds, small amounts of pyro-, isopyro-, and iso-vitamin D and isotachysterol3 variants were obtained from each Vitamin D-related compound upon extraction and GC/MS/MS analysis. Mass spectral and chromatographic behavior of these compounds are herein described and interpreted. Multiple Reaction Monitoring settings on GC/MS/MS included m/z 456→351 for Vitamin D3 and m/z 486→363 for Vitamin D2. Trimethylsilylation enabled single predominant peaks for Vitamins D3 and D2, and sample workup in the presence of deuterated Vitamin D analogs enabled accurate and precise sensitivity to 1 ppb (ng/g) in feeds. The method could be extended with reasonable accuracy to 25-hydroxy (25OH) compounds, but accuracies would be significantly improved by inclusion of respective 25OH-specific deuterated internal standards. The method was applied to 27 submissions of suspect dog foods of which 22% were discovered elevated and 44% were discovered to contain toxic levels of Vitamin D3. The described method was thus discovered to provide a suitable mass spectrometric approach for Vitamin D, proving itself here specifically of value in detection of ergocalciferol and cholecalciferol in animal feeds. The specificity and sensitivity of the tandem quadrupole approach can enable suitable applicability to serum determination if desired.

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Rapid determination of vitamin D3 in milk-based infant formulas by liquid chromatography-tandem mass spectrometry

Cited by 20 publications

References 14 publications

Quantification of selected fat soluble vitamins and carotenoids in infant formula and dietary supplements using fast liquid chromatography coupled with tandem mass spectrometry

Quantification of selected fat soluble vitamins and carotenoids in infant formula and dietary supplements using fast liquid chromatography coupled with tandem mass spectrometry

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

Vitamin D analyses in veterinary feeds by gas chromatography-tandem mass spectrometry

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