• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.5
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• pp.716-724
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• 2015

Trienzyme extraction coupled with microplate assay (Lactobacillus casei subsp. rhamnosus) was validated and applied for the determination of folate (vitamin B9) in Korean ancestral rite foods. Foods included five Guk (Tang), eleven Sookchaes, eight Jeoks, nine Jeons, six Jjims, and twenty desserts. Folate was detected in all samples: Guk (Tang) 4.62~18.84, Sookchae 6.13~48.40, Jeok 5.49~49.50, Jeon 6.96~30.77, Jjim 10.34~38.88, and desserts $3.33{\sim}49.55{\mu}g/100g$. The lowest folate content was observed in Sikhye ($3.33{\mu}g/100g$), whereas the highest was observed in Songhwa-dasik ($49.55{\mu}g/100g$). Folate analyses of certified reference materials, BCR-121 (whole meal flour) and BCR-487 (pig liver), showed good recoveries of 90.0% (0.45 mg/kg) and 92.4% (12.3 mg/kg), respectively. The recoveries (96.0 to 106.2%) obtained by analyzing eight spiked samples with different matrices also showed good accuracy. Both repeatability and reproducibility were less than 5%, indicating good precision. The quality control chart (n>30) obtained by running commercial folate fortified-wheat flour once a week for about 10 months showed that all assays were under control. All validation method and analytical quality control results showed that folate contents in Korean ancestral rite foods produced by microplate assay were reliable enough to be used for the construction of a national folate database.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.411-417
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• 2017

This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.

• Korean Journal of Environmental Agriculture
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• v.30 no.3
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• pp.288-294
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• 2011

BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at $60^{\circ}C$ in microwave for 20 min. Methylmercury in $50{\mu}L$ of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at $25^{\circ}C$. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient($r^2$) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and $0.45{\mu}g/kg$ respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.