Overview
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Key numbers
The worker extracted the full PDF text with layout preservation twice and compared extraction hashes before commit. The following lines are copied from numeric/table-bearing regions of the PDF and retain the source units and wording where legible:
- The analyte was separated isocratically on a C-8 column in under 6 minutes using a mobile phase of 0.1% (v/v) formic acid in
- (< 14% RSD) was demonstrated by interday analysis of samples and reference materials. Recovery values mostly ranged
- between 80% and 120% for fortified samples and reference materials. Vitamin B12 can be detected and quantified using the
- functioning of the brain and nervous system (Allen 2012). Its 2024). The synthetic and chemically stable form of cobala-
- spectrophotometry, and liquid chromatography coupled with glacial acetic acid (99%), hydrogen peroxide solution (H2O2,
- ultraviolet detection (LC-UV), many of which are limited in 30–32%), and sodium cyanide (98%) were purchased from
- most official (AOAC 1960, 2014) and other methods (Amrit- Baker Chemicals, and trifluoroacetic acid (≥ 99.5%) from
- viding sensitive, selective, and robust detection. Coupling was discarded if the OHCbl peak was > 2% relative to the
- The present study aimed to develop an HPLC-ICP-MS cereals, was purchased from local stores (Table 1).
- liporeSigma. Optima grade nitric acid (HNO3, 67–70%), post-column marker
- Table 1 List of samples with their label claim and measured vitamin B12 mass fractions
- and d% daily value/serving size; e%RSD for measured vitamin B12 mass fraction (n = 3)
- disposable grinding chambers and then preserved in amber isopropanol. See Table 2 for the ICP-MS operating conditions.
- Option gas mixd 20%c
- Mobile phases 0.1% formic acid in (A) water and (B) methanol
- Isocratic 0–6.0 min (30% B)
- Column was rinsed with 95% (v/v) methanol for 20–30 min at the start of every analytical batch; fresh col-
- Eight extraction methods described in Table 3 were evalu- the tube by forcing air with a syringe. The SPE eluate was
- tion and vortexed for 30 seconds. For methods other than mL of 0.1% (v/v) formic acid in water for subsequent analy-
- M4 and M5, starch-containing samples were treated with sis by HPLC-ICP-MS (Table 2). Solvents and extracts were
- analyzed by HPLC-ICP-MS (Table 2). An ultrasonic cleaner Depending on the expected level of vitamin B12, a 0.5–2.0
- Table 3 Extraction methods evaluated
- M4 Acetic acid, 1% (v/v) Sonicate, ambient 15 min (D’Ulivo et al. 2017)
- M5 Nitric acid, 1% (v/v) Sonicate, ambient 15 min (Chen and Jiang 2008)
- cyanide, 1% (w/v)d
- 250 µL of 1% (w/v) sodium cyanide in 10-mL acetate buffer
- two-component mobile phase of 0.1% (v/v) formic acid uct listed in Table 1 over the course of three days. The
- in methanol and water (30:70). The ICP-MS was operated three-tiered spikes corresponded to 50% (low level), 100%
- in O2/Ar option gas mode to oxidize the high amounts of (medium level), and 150% (high level) of the native analyte
- ions such as 24Mg 35Cl, 43Ca 16O, and 23Na 36Ar on Co at tification (LOQ) of the method. Samples were fortified after
- that the ISTD eluted before the void. Table 2 shows the matched reference material(s).
- Waters Empower 3 Chromatography Data software was time. Formic acid (0.1% v/v) was added to ensure retention
- of matrices, the extraction methods described in Table 3 fere in analyte enrichment on SPE sorbent. In all the extrac-
- were evaluated by analyzing reference materials of infant/ tion procedures listed in Table 3, except for acidic extrac-
- fast cereal (SRM 3233). matrix. All extracts from the methods in Table 3 were ana-
- Fortified CNCbl can easily be solubilized through mild lyzed using the HPLC-ICP-MS method described in Table 2.
- assessed via sonication as described in Table 3 (M1–M3). lyzed using an HPLC-ICP-MS method that separates the
- molecular hydrolysis at moderate temperatures maintaining ods in Table 3. Recoveries could not be determined for some
- described in Table 3 (n = 2).
- Huang et al. 2022; Pakin et al. 2005), as well as breakfast in the extracts in those days ranged between 0.1 and 6.3%,
- rials (n = 2)
- Single Laboratory Validation over three days (n = 3). Table 1 summarizes the average
Methods (brief)
- Measurement in Nutritional Products by HPLC‑ICP‑MS
- solid phase extraction (SPE) sorbent. Starch-containing samples were treated with α-amylase (300 µL) and incubated (40 °C,
- high-performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS).
- (< 14% RSD) was demonstrated by interday analysis of samples and reference materials. Recovery values mostly ranged
- between 80% and 120% for fortified samples and reference materials. Vitamin B12 can be detected and quantified using the
- current method at levels as low as 0.004 and 0.03 µg CNCbl/100 g (liquid and ready-to-feed/drink samples) and 0.01 and
- 0.06 µg CNCbl/100 g (solid samples), respectively. The method is simpler and less time-consuming than most official and
- Keywords Vitamin B12 · Nutritional products · HPLC-ICP-MS · Validation
- sensitivity and specificity, and/or laborious and time-con- Fisher Scientific. HPLC grade methanol and acetonitrile,
- milk. The determination of vitamin B12 in nutritional prod- analysis by HPLC-ICP-MS.
- for selective detection using techniques normally dedicated ard was analyzed by ICP-MS to verify the total Co mass
- spectrometry (ICP-MS) is best suited for such analyses, pro- monitoring the formation of OHCbl (Fig. 1); the solution
- high-performance liquid chromatography (HPLC) to ICP- CNCbl peak. Due to their lack of stability, the solutions of
- of HPLC-ICP-MS has been used to determine vitamin B12 stored under subdued light or in amber tubes.
- 2014; Zhang et al. 2008) and biological matrices (Bosle Samples and Reference Materials
- The present study aimed to develop an HPLC-ICP-MS cereals, was purchased from local stores (Table 1).
- and breakfast cereals. Sample preparation was based on liq- milk powder (1549a), soy milk (3235), protein drink
- on samples and reference materials covering a wide range
Implications
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Wiki pages this source may touch
- Infant Formula Powder
- Fish — marine, non-predatory (sardines, anchovies, salmon, cod)
- Root-Vegetable Purees
- Mercury
- Cadmium
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- Chromium
Verification notes
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Update history
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