Enzymatic extraction of anthocyanins from the pomace of aronia (Aronia melanocarpa).

Efficient extraction of natural pigments is a key focus in enhancing the utilization of by-products for applications in the food industry. In this study, an enzymatic extraction method using Pectinex Ultra SP-L, Pectinex XXL, Novoshape, and Celluclast was used to investigate natural pigment production from the pomace of aronia, a commercially important plant. The method's performance was monitored using high-performance liquid chromatography with diode-array detection by measuring total and individual anthocyanin levels. Pectinex XXL (0.5%) yielded the highest total anthocyanin extraction (2082.41 ± 85.69 mg/100 g) in the single enzyme treatment, followed by Pectinex Ultra SP-L (0.05%), Celluclast (0.01%), and Novoshape (0.1%). Combining Pectinex XXL (0.25%) with Celluclast (0.01%) increased the extraction ratio of total anthocyanins (2 323.04 ± 61.32 mg/100 g) by ∼50.7% compared with that obtained using the solvent extraction method. This study demonstrated an effective enzymatic extraction method for application in the food industry.

ß-Carotene and ß-apo-8'-carotenal contents in processed foods in Korea.

A robust and rapid HPLC method for ß-carotene and ß-apo-8'-carotenal analyses in various processed foods was developed. The analysis method was validated for low-fat, moderate-fat, and high-fat food matrices. The two carotenoids were identified by LC-MS/MS. The detection limits for ß-carotene and ß-apo-8'-carotenal in the three food matrices were 0.08-0.27 µg/g and 0.09-0.18 µg/g, respectively. The inter- and intra-day accuracy and precision were in accordance with the Codex guidelines. The validated method was applied to 57 processed food samples, possibly containing ß-carotene and ß-apo-8'-carotenal, obtained in Korea. The detected ß-carotene and ß-apo-8'-carotenal levels in the samples ranged from not detected (ND) to 6.92 µg/g and ND to 1.63 µg/g, respectively. Chocolate and cheese samples had the highest ß-carotene and ß-apo-8'-carotenal levels, respectively. Notably, several samples with no labeled carotenoid additives contained ß-carotene. Moreover, the developed analytical method was compatible with various processed food matrices. Supplementary Information: The online version contains supplementary material available at 10.1007/s10068-023-01285-2.

High-performance liquid chromatography using diode array detector and fluorescence detector for hydrogen peroxide analysis in processed fishery foods.

Hydrogen peroxide (H2O2) is a food additive for bleaching and sterilization, owing to its strong oxidizing effect. The current study aimed to develop analytical methods to detect trace amounts of residual H2O2 in diverse foods using high-performance liquid chromatography (HPLC) equipped with diode array detector (DAD) or fluorescence detector (FLD). The vanadium(V)-peroxo complex, derived from the reaction of H2O2 with ammonium metavanadate, was used for the detection of H2O2 with DAD. H2O2 was indirectly analyzed using FLD via the detection of 7-hydroxycoumarin, derived by Fenton reaction, followed by verification using liquid chromatography with tandem mass spectrometry analysis. Both the detection methods showed good linearity with R2 > 0.997. Limit of detection and limit of quantification were 0.30 and 0.91 mg/L (8.82 and 26.76 µM) with HPLC-DAD and 0.001 and 0.003 mg/L (0.03 and 0.09 µM) with HPLC-FLD, respectively. Applicability of both the methods was successively tested through sample analysis.

A high-performance liquid chromatography-evaporative light scattering detection-based quantitative analytical method for polyvinyl alcohol in food supplements with pyrolysis-gas chromatography/mass spectrometry-based verification.

Polyvinyl alcohol (PVOH) is extensively used in agricultural, pharmaceutical, textile, and food industries. A new high-performance liquid chromatography (HPLC) method with evaporative light scattering detection (ELSD) was developed for the quantitative analysis of PVOH products. Pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was employed for method verification. The HPLC-ELSD method exhibited acceptable linearity (R2 > 0.99), with limits of detection and quantitation of 19.43 and 58.88 µg/mL, respectively. Accuracies of 91.16-102.30% were estimated based on recoveries of the intra- and inter-day tests of PVOH. Repeatability and intermediate precision (%RSD) of 1.23-4.45 and 2.18-6.95, respectively, were obtained. The presence of PVOH in the HPLC peaks was further verified using typical indicators of PVOH in Py-GC/MS analysis, such as acetaldehyde, 2,5-dihydrofuran, benzaldehyde, and crotonaldehyde. This novel HPLC method with Py-GC/MS-based verification can be successfully applied for analyzing PVOH in dietary supplement tablets.

Determination of Polyvinyl Acetate in Chewing Gum Using High-Performance Liquid Chromatography-Evaporative Light Scattering Detector and Pyrolyzer-Gas Chromatography-Mass Spectrometry.

Polyvinyl acetate (PVAc) is used in various adhesive, paint, and transparent tape applications. It is also used as a food additive in food manufacturing to make chewing gum and fruit and vegetable glazes; however, guidelines on the amount of food additives that is used have not yet been established. In this study, a method was developed for analysis of polyvinyl acetate (PVAc) using high-performance liquid chromatography with an evaporative light scattering detector (HPLC-ELSD) and pyrolyzer-gas chromatography-mass spectrometry (Py-GC-MS). The analytical methods were applied to commercially available chewing gum. In the HPLC-ELSD analysis, the linearity was acceptable (R2 > 0.999), and the limits of detection and quantification were 22.2 and 67.3 µg/mL, respectively. The accuracies of PVAc were 87-115% at spike levels of 200-1000 µg/mL for the intra- and inter-day tests. The contents of PVAc in the chewing gum samples were n.d. (not detected)-13.8 g/kg. The presence of PVAc in chewing gum was verified with Py-GC-MS analysis, finding the typical pyrolysates of PVAc, such as acetic acid, benzene, toluene, styrene, indane, naphthalene, and acenaphthene. The developed analytical methods can be applied for successful identification of PVAc in chewing gum.

Quantification of Morpholine in Peel and Pulp of Apples and Oranges by Gas Chromatography-Mass Spectrometry.

Morpholine salts of fatty acids have been used in wax coatings on the surfaces of fruit and vegetable commodities in China and the United States, etc. However, morpholine usage was prohibited in many other countries because of safety concerns. We optimized analytical methods to determine morpholine in the peel and pulp of fruits and vegetables by gas chromatography-mass spectrometry (GC-MS). This morpholine analysis method was applied to real samples of apples, citrus fruits, and vegetables from Korea, China, and the U.S. The method was validated using apple and citrus fruit peels and pulp. The method detection limit (MDL) was 1.3-3.3 µg/kg. The recovery rates of morpholine were 88.6-107.2% over a fortified level of 10-400 µg/kg. Intra-day and inter-day precisions were 1.4-9.4% and 1.5-2.8%, respectively. The morpholine concentrations were n.d. (not detected)-11.19 and n.d. (not detected)-12.82 µg/kg in apple and citrus peels, respectively. Morpholine was not detected in citrus or apple pulp samples or in vegetable samples.

Simultaneous analysis of polyethylene glycol in dietary supplement tablets using high-performance liquid chromatography and verification with liquid chromatography-electrospray ionization mass spectrometry.

Polyethylene glycol (PEG) are widely applied in detergents, cosmetics, and food additives. A simultaneous analytical method was developed to detection the polyethylene glycol (100-10000 Da). High-performance liquid chromatography (HPLC) with evaporative light scattering detector (ELSD) could analyze successively PEG products. The method was verified with liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS/MS). The retention times of PEG 200-8000 ranged from 1.97 to 12.33 min. Method validation was performed to the International Conference on Harmonization (ICH) guidelines and the Korea Ministry of Food and Drug Safety (MFDS); linearity: R2 > 0.997, LOD: 7.47-16.24 µg/mL, LOQ: 22.40-75 µg/mL, repeatability (%RSD): 0.2-2.5, recovery (%): 90.4-104.9% for film-coated tablet, 80.1-95.9% for sugar-coated tablet. A total of 115 PEG could be identified by extracted ion chromatography in mass analysis, based on the charge state represented as [M+Na++H3O+n-1]. This method can be applied for successive identification of PEGs in PEG-containing products.

High-performance liquid chromatography and gas chromatography to set the analysis method of stearoyl lactylate, a food emulsifier.

Stearoyl lactylates (SLs, E481/E482) and their sodium and calcium salts are emulsifiers commonly used as food additives. This study was performed to set the analytical method of SLs in Korea using high-performance liquid chromatography (HPLC) and gas chromatography (GC). A new HPLC method using C18 column with water and methanol as the eluents, and a new GC method using DB-1 column with He as the carrier gas, were developed and were compared with previously reported analytical methods. The new HPLC and GC methods indicated a coefficient of determination (r2) of 0.999 in the calibration curves. The detection and quantification limits are 0.26 and 0.78 µg/kg for the HPLC method, respectively, and 16.54 and 50.12 µg/kg for the GC method, respectively. The new HPLC and GC methods indicated precision of 0-2.0%, and accuracy of 92.7-108.5%. Therefore, they can be applied in numerous food samples to determine the level of SLs.

Simultaneous determination of sodium iron chlorophyllin and sodium copper chlorophyllin in food using high-performance liquid chromatography and ultra-performance liquid chromatography-mass spectrometry.

A simultaneous method for analyzing sodium iron chlorophyllin (SIC) and sodium copper chlorophyllin (SCC) using high-performance liquid chromatography was developed. This method employed an Inertsil ODS-2 column and diode array detection at 395 nm, using methanol-water (97:3 and 80:20, v/v) containing 1% acetic acid as the mobile phase. Liquid chromatography-tandem mass spectrometry was used to identify the main components of SIC and SCC as Fe-isochlorine e4 and Cu-isochlorine e4, respectively. The limits of detection and quantitation of SIC were 1.2 and 4.1 mg/kg, respectively, while those of SCC were 1.4 and 4.8 mg/kg, respectively. For intraday and interday tests, the SIC recoveries from candy ranged from 81% to 101%, while SCC recoveries ranged from 100% to 109%. The developed method can be applied to the rapid determination of SIC and SCC in candy.

An Improved Analytical Method for the Determination of Brown FK in Food using HPLC.

In this study, an improved analytical method for the detection of the colorant Brown FK in foods using high-performance liquid chromatography was developed. The method, which employed an RC-C18 column and diode array detection at 254 nm with sodium acetate solution and methanol as mobile phases, exhibited good linearity (R2 = 1.0), and its limits of detection and quantification were determined to be 0.06 and 0.19 µg/mL, respectively. The precision was found to be 0-1.2% and the accuracy was between 86.5% and 94.8%. Liquid chromatography-tandem mass spectrometry was also performed to identify Brown FK in peaks. The pretreatment method was optimized for three different food sample groups, i.e., seafood, noodles and other, affording recoveries of 86.5-92.8%, 90.8-94.8% and 90.0-92.3%, respectively. In addition, inter-laboratory testing was also conducted to check the precision.

Under-reporting of Energy Intake from 24-hour Dietary Recalls in the Korean National Health and Nutrition Examination Survey.

OBJECTIVES: Chronic degenerative diseases are closely related to daily eating habits, nutritional status, and, in particular, energy intake. In clarifying these relationships it is very important for dietary surveys to report accurate information about energy intake. This study attempted to identify the prevalence of the under-reporting of energy intake and its related characteristics based on the Korean National Health and Nutrition Examination Survey conducted in the years 2007-2009. METHODS: The present study analyzed dietary intake data from 15,133 adults aged ≥19 years using 24-hour dietary recalls. Basal metabolic rates were calculated from the age- and gender-specific equations of Schofield and under-reporting was defined as an energy intake <0.9, represented by the ratio of energy intake to estimated basal metabolic rate. RESULTS: Under-reporters (URs) accounted for 14.4% of men and 23.0% of women and the under-reporting rate was higher in the age group 30-49 years for both men and women. The results from an analysis of the age-specific socioeconomic characteristics of participants classified as URs showed that under-reporting was high in women living alone and in women with only elementary school education or no education. The results from an analysis of the health-specific characteristics of URs showed that a large proportion of URs had poor self-rated health or were obese, or both, compared with non-URs. The proportion of participants who consumed less than the estimated average requirements for nutrients was significantly higher in URs compared with non-URs. CONCLUSION: The under-reporting of energy intake was associated with age, gender, education level, income level, household status (single-person or multi-person), self-rated health, physical activity, and obesity.

Breakfast eating patterns and the metabolic syndrome: the Korea National Health and Nutrition Examination Survey (KNHANES) 2007-2009.

OBJECTIVE: The purpose of this study is to find out the association between eating breakfast, breakfast patterns, and the metabolic syndrome. METHODS: We used the fourth Korean National Health and Nutrition Examination Survey from 2007 to 2009. A total of 16,734 subjects were included. Breakfast dietary patterns were extracted by factor analysis. Multiple logistic regression was used to assess the relationship between breakfast consumption, breakfast dietary patterns, and the metabolic syndrome. RESULTS: We found that breakfast consumption itself reduced the risk of the metabolic syndrome (odds ratio=0.82, 95% confidence interval=0.69-0.98). We identified two breakfast dietary patterns: the traditional Korean pattern and the dairy-cereal pattern. The dairy-cereal pattern was associated with a reduction in the risk of the metabolic syndrome among breakfast consumers. Compared to no breakfast consumption, the strongest traditional Korean pattern and the highest quartiles for the dairy-cereal pattern were associated with a reduced risk of the metabolic syndrome. CONCLUSIONS: Breakfast consumption is associated with the metabolic syndrome. Not all breakfast consumption patterns are associated with a reduced risk of having the metabolic syndrome. In particular, eating either a dairy-cereal breakfast or high energy and fiber breakfast are associated with a reduced risk of the metabolic syndrome.