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KMID : 0881720160310050327
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Journal of Food Hygiene and Safety
2016 Volume.31 No. 5 p.327 ~ p.334
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Establishment of Biotin Analysis by LC-MS/MS Method in Infant Milk Formulas
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Shin Yong-Woon
Lee Hwa-Jung
Ham Hyeon-Suk
Kang Yoon-Jung
Hwang Kyung-Mi
Kwon Yong-Kwan
Seo Il-Won
Oh Jae-Myoung
Koo Yong-Eui
Shin Sung-Cheol
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Abstract
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This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using C18 column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 → 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over R2 = 0.999 in range of 5~60 μg/L. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.
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KEYWORD
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biotin, LC-MS/MS, milk formula, method validation
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