Jang-Hyuk Ahn

Method validation for simultaneous determination of chromium, molybdenum and selenium in infant formulas by ICP-OES and ICP-MS

This study aimed to validate the analytical method for simultaneous determination of chromium (Cr), molybdenum (Mo), and selenium (Se) in infant formulas available in South Korea. Various digestion methods of dry-ashing, wet-digestion and microwave were evaluated for samples preparation and both inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were compared for analysis. The analytical techniques were validated by detection limits, precision, accuracy and recovery experiments. Results showed that wet-digestion and microwave methods were giving satisfactory results for sample preparation, while ICP-MS was found more sensitive and effective technique than ICP-OES. The recovery (%) of Se, Mo and Cr by ICP-OES were 40.9, 109.4 and 0, compared to 99.1, 98.7 and 98.4, respectively by ICP-MS. The contents of Cr, Mo and Se in infant formulas by ICP-MS were found in good nutritional values in accordance to nutrient standards for infant formulas CODEX values.

Three-configurational surface magneto-optical Kerr effect measurement system for an ultrahigh vacuum in situ study of ultrathin magnetic films

We have constructed a three-configurational surface magneto-optical Kerr effect system, which provides the simultaneous measurements of the “polar,” “longitudinal,” and “transverse” Kerr hysteresis loops at the position where deposition is carried out in an ultrahigh vacuum growth chamber. The present system enables in situ three-dimensional vectorial studies of ultrathin film magnetism with a submonolayer sensitivity. We present three-configurational hysteresis loops measured during the growth of Co films on Pd(111), glass, and Pd/glass substrates.

Rapid determination of cholesterol in milk containing emulsified foods.

In this study, a rapid and easy sample preparation method that involved no-heating saponification and dSPE (dispersive solid phase extraction) clean-up was developed to determine the level of cholesterol in milk containing emulsified foods (infant formula, baby food, cheese). The developed method utilised high performance liquid chromatography with an ultraviolet detector (HPLC-UVD) as a separation instrument. The optimum extraction conditions were determined as 10 mL isopropyl alcohol with 8.0 g (NH(4))(2)SO(4) per 1g sample, and saponification was achieved using 25mg KOH, 1.6g NaCl and 100mg of a silica based NH(2). Cholesterol levels determined using CRMs (NIST SRM 1849 and 1544) were in the range of the certificated value and the recovery test using spiked materials ranged from 94.34% to 102.34% with a RSD of 0.63-4.10%. This method enables the accurate determination of cholesterol with reduced sample preparation time.

Determination of Isomaltooligosaccharides in Yoghurts by Using HPLC-ELSD

A rapid and simple analytical method for the determination of 9 isomaltooligosaccharides (IMO) species in yoghurts was developed using dispersive solid phase extraction (dSPE) clean-up technic and high performance liquid chromatography with evaporative light-scattering detector (HPLC-ELSD). In this study, 9 IMO were extracted from samples simply with chemical reagent using ISO22662 IDF198 method and additional dSPE clean-up. The optimum instrument conditions for the determination were used carbohydrate ES 5µ column with gradient elution of water and acetonitrile and ELS detector. The linearity of this method was expressed as the correlation coefficient (r 2 ), the results of IMO 9 species were shown in 0.9999. LOD and LOQ were respectively 7.9-22.1 mg/kg, 25.9-72.8 mg/kg. The accuracy of intra- and inter-day measurements were in the range from 84.3±4.5 to 104.9±6.5%, and the preceision of the intra- and inter-day measurements were in the range from 0.8 to 7.7%. The recoveries were from 84.3±4.5 to 104.9±6.5%. The determination results of IMO 9 species for the 9 yoghurts circulated in the market were in the range from 0.317±0.007 to 1.624±0.050 g/100 g. The newly developed method is appropriate for the determination of IMO in yoghurts, is a rapid and simple method with excellent resolution in compared with previous method.

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

A rapid and simple sample preparation method for vitamin D3 (cholecalciferol) was developed for emulsified dairy products such as milk-based infant formulas. A sample was mixed in a 50 mL centrifuge tube with the same amount of water and isopropyl alcohol to achieve chemical extraction. Ammonium sulfate was used to induce phase separation. No-heating saponification was performed in the sample tube by adding KOH, NaCl, and NH3. Vitamin D3 was then separated and quantified using liquid chromatography-tandem mass spectrometry. The results for added recovery tests were in the range 93.11-110.65%, with relative standard deviations between 2.66% and 2.93%. The results, compared to those obtained using a certified reference material (SRM 1849a), were within the range of the certificated values. This method could be implemented in many laboratories that require time and labour saving.

Rapid Determination of L-carnitine in Infant and Toddler Formulas by Liquid Chromatography Tandem Mass Spectrometry.

A rapid and simple analytical method for L-carnitine was developed for infant and toddler formulas by liquid chromatography tandem mass spectrometry (LC-MS/MS). A 0.3 g of infant formula and toddler formula sample was mixed in a 50 mL conical tube with 9 mL water and 1 mL 0.1 M hydrochloric acid (HCl) to chemical extraction. Then, chloroform was used for removing a lipid fraction. After centrifuged, L-carnitine was separated and quantified using LC-MS/MS with electrospray ionization (ESI) mode. The precursor ion for L-carnitine was m/z 162, and product ions were m/z 103 (quantitative) and m/z 85 (qualitative), respectively. The results for spiked recovery test were in the range of 93.18-95.64% and the result for certified reference material (SRM 1849a) was within the range of the certificated values. This method could be implemented in many laboratories that require time and labor saving.

Sensitive and multiplexed analysis of aflatoxins using time-of-flight secondary ion mass spectrometry

A rapid and reliable analysis of toxins is prerequisite for food control and human healthcare. Here we demonstrate a simple and multiplexed assay of aflatoxins using time-of-flight secondary ion mass spectrometry (TOF-SIMS). By simply adsorbing either a single analyte or mixed ones onto a gold substrate, the corresponding secondary molecular ions([M+H]+) were clearly observed in a single mass spectrum. As a result of concentration-dependent peak intensity, quantitative and multiplexed analysis of different aflatoxin analogs from corns was accomplished with immunoaffinity column and TOF-SIMS analysis, which showed a good correlation with HPLC data. The detection sensitivity was estimated to be as low as 10 ng mL−1. This approach presented here will find a wide application to detection of low-levels of toxins in a rapid and multiplexed way.

Analytical Determination of Vitamin B12 Content in Infant and Toddler Milk Formulas by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

The development of a sample preparation method and optimization of the analytical instrumentation conditions were performed for the determination of the vitamin B12 content in emulsified baby foods sold on the Korea market. After removal of the milk protein and fats by chloroform extraction and centrifugation, the vitamin B12 was water extracted from the sample. Following filtration of the solution through a nylon filter, the water-soluble extract was purified by solid-phase extraction using a Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS). The solution eluted from the cartridge was dried under a stream of nitrogen gas and reconstituted with 1 mL of water. The sample solution was injected into an LC-MS/MS system after optimizing the mobile phase for vitamin B12 detection. The calibration curve showed good linearity with the coefficient of correlation (r2) value of 0.9999. The limit of detection was 0.03 µg/L and the limit of quantitation was 0.1 µg/L. The method of detection limit was 0.02 µg/kg. The vitamin B12 recovery from a spiking test was 99.62% for infant formula and 99.46% for cereal-based baby food. The sample preparation method developed in this study would be appropriate for the rapid determination of the vitamin B12 content in infant formula and baby foods with emulsified milk characteristics. The ability to obtain stable results more quickly and efficiently would also allow governments to exercise a more extensive quality control inspection and monitoring of products expected to contain vitamin B12. This method could be implemented in laboratories that require time and labor saving.

Development Rapid Analytical Methods for Inositol as a Trace Component by HPLC and LC-MS/MS in Infant Formula

A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

Simultaneous Determination of Synephrine and N-Methyltyramine in Orange Fruit and Juice from Korean Market by UPLC-FLD

An accurate and sensitive analytical method was established for the simultaneous determination of synephrine and n-methyltyramine contents by ultra-performance liquid chromatography (UPLC) with a fluorescence detector (FLD). A 70:30 (v/v) mixture of 10 mM sodium dodecyl sulfate (SDS) and acetonitrile was used as the mobile phase. The coefficient of correlation (r 2 ) was 0.9999 for both synephrine and n-methyltyramine, and their limits of detection (LOD) were 0.02 and 0.01 mg/kg, respectively. The percentage recoveries for synephrine and n-methyltyramine were 96.4% and 100.9%, respectively, from bitter orange (Citrus aurantium) samples. The synephrine and n-methyltyramine contents were 38.07-118.21 mg/kg and 0.27-0.56 mg/kg, respectively, in the orange fruit samples, while they were 14.61-120.39 mg/kg and up to 3.34 mg/kg, respectively, in the tested commercial orange juice samples. The differences in synephrine and n- methyltyramine content between orange fruit and commercial orange juice were not significant (p<0.05). These results suggest that UPLC-FLD can be applied to develop an analytical method of quality control for commercial orange juice.