Determination of alcohols in various fermented food matrices using gas chromatography-flame ionization detector for halal certification.

In this study, an analytical method for the determination of alcohols by gas chromatography-flame ionization detection was applied to fermented foods. The limit of detection and limit of quantitation were 0.79 and 2.40 mg/kg for methanol, 0.55 and 1.66 mg/kg for ethanol, 0.51 and 1.56 mg/kg for n-propanol, 0.35 and 1.05 mg/kg for n-butanol, and 0.38 and 1.16 mg/kg for n-pentanol, respectively. The recoveries from the matrices of gochujang, soy sauce, and kimchi were 93.80-102.03%, 93.27-99.69% and 89.06-102.17%, respectively, and the corresponding intra- and inter-day relative standard deviations were below 5.33%, 5.35% and 4.10%. In 95 fermented foods, ethanol showed the highest mean, median and maximum values among the five alcohols. The detection rate of ethanol was 86.3% among all samples and 100% in gochujang and gochujang-based sauces. A total of 22 samples had an alcohol content above 0.5%, of which 16 were gochujang.

Determination of Indicators for Dry Aged Beef Quality.

Previous studies on dry aged beef, which substantially increases the value of low-grade raw beef and non-preferred cuts, are currently limited to the observation of aged beef changes in laboratory settings or under particular aging conditions, whereas the factors influencing aging have so far been underexplored. Herein, we attempt to establish a technique for distinguishing between fresh and aged beef by observing changes in quality during beef aging. Specifically, we analyzed the effect of time on the quality of aged beef sourced from three Korean manufacturers and identified quality indicators that can be used to distinguish between fresh and aged beef, regardless of supplier. Storage/trimming/aging/cooking losses, moisture/fat/protein/collagen contents, and water holding capacity were tested as potential indicators, among other parameters. As a result, the quality of dry aged beef was shown to be supplier-dependent, which made the identification of factors for the above origin-independent discrimination difficult. Nevertheless, as storage loss, water holding capacity, and cooking loss significantly changed with dry aging time in all cases, these parameters were concluded to be potentially suited for discrimination purposes. The insights gained in this work may help promoting further research in this field and contribute to the development of a standard for consistent aged beef production.

Simultaneous Determination of Piperine, Capsaicin, and Dihydrocapsaicin in Korean Instant-Noodle (Ramyun) Soup Base Using High-Performance Liquid Chromatography with Ultraviolet Detection.

A simultaneous analytical method for piperine, capsaicin, and dihydrocapsaicin in Korean instant-noodle soup base using HPLC was validated in terms of precision, accuracy, sensitivity, and linearity. The HPLC separation was performed on a reversed-phase C18 column (5 µm particle size, 4.6 mm id, 250 mm length) using a UV detector fixed at 280 nm. The LOD and LOQ of the HPLC analyses ranged from 0.25 to 1.03 mg/kg. The intraday and interday precisions of the individual piperine, capsaicin, and dihydrocapsaicin were <10.55%, and the recovery values ranged from 85.43 to 94.68%. The calibration curves exhibited good linearity (r(2) = 0.999) within the tested ranges. These results suggest that the analytical method in this study can be used to classify Korean instant noodles based on their levels of spiciness.

Method validation of analytical method for 12 flavonol glycosides in foods using ultra high-performance liquid chromatography coupled with photodiode array detection.

An analytical method for the simultaneous determination of 12 flavonol glycosides in buckwheat, black tea, and wild parsley using ultra high-performance liquid chromatography (UHPLC) coupled with a simple liquid extraction method using dimethyl sulfoxide (DMSO) was validated in precision, accuracy, and linearity. The UHPLC separation of target compounds was performed on a C18 column using a photodiode array (PDA) detector and the wavelength was fixed at 350 nm. The recovery values for flavonol glycosides ranged from 85.44 to 108.79%. The limits of detection and limits of quantification were less than 0.32 mg/kg and less than 0.97 mg/kg, respectively. The intraday and interday precisions were less than 13.69% for all the test samples. This method coupled with UHPLCPDA detection could be expected to provide more convenient sample preparation than conventional methods in the tested foods.

The simple determination method for anthocyanidin aglycones in fruits using ultra-high-performance liquid chromatography.

The simple determination method for anthocyanidin aglycones in fruits using ultra-high-performance liquid chromatography (UHPLC) coupled with the heating-block acidic hydrolysis method was validated through the precision, accuracy and linearity. The UHPLC separation was performed on a reversed-phase C18 column (particle size 2 µm, i.d. 2 mm, length 100 mm) with a photodiode-array detector. The limits of detection and quantification of the UHPLC analyses were 0.09 and 0.29 mg/kg for delphinidin, 0.08 and 0.24 mg/kg for cyanidin, 0.09 and 0.26 mg/kg for petunidin, 0.14 and 0.42 mg/kg for pelargonidin, 0.16 and 0.48 mg/kg for peonidin and 0.30 and 0.91 mg/kg for malvidin, respectively. The intra- and inter-day precisions of individual anthocyanidin aglycones were <10.3%. All calibration curves exhibited good linearity (r = 0.999) within the tested ranges. The total run time of UHPLC was 8 min. The simple preparation method with UHPLC detection in this study presented herein significantly improved the speed and the simplicity for preparation step of delphinidin, cyanidin, petunidin, pelargonidin, peonidin and malvidin in fruits. Especially, the UHPLC detection exhibited good resolution in spite of shorter run time about four times than conventional HPLC detection.

Rapid method for the determination of 14 isoflavones in food using UHPLC coupled to photo diode array detection.

A rapid method for the determination of 14 types of isoflavones in food using ultra-high performance liquid chromatography (UHPLC) was validated in terms of precision, accuracy, sensitivity and linearity. The UHPLC separation was performed on a reverse-phase C18 column (particle size 2 µm, i.d. 2 mm, length 100 mm) using a photo diode array detector that was fixed to 260 nm. The limits of detection and quantification of the UHPLC analyses ranged from 0.03 to 0.33 mg kg(-1). The intra-day and inter-day precision of the individual isoflavones were less than 11.77% and calibration curves exhibited good linearity (r(2) = 0.99) within the tested ranges. These results suggest that the rapid method used in this study could be available to determine of 14 types of isoflavones in a variety of food such as soy bean, black bean, red bean and soybean paste.

Rapid method for determination of anthocyanin glucosides and free delphinidin in grapes using u-HPLC.

A rapid method for the determination of anthocyanin glucosides and free delphinidin in food using ultra-high-performance liquid chromatography (u-HPLC) was validated through tests of precision, accuracy and linearity. The u-HPLC separation was performed on a reversed-phase C18 column (particle size 2 µm, i.d. 2 mm, length 100 mm) with a photodiode array detector. The limits of detection and quantification of the u-HPLC analyses ranged from 0.07 to 0.65 mg/kg for nine types of anthocyanin glucosides and from 0.08 to 0.26 mg/kg for delphinidin aglycone. The intra-day and inter-day precision of individual anthocyanin glucosides and delphinidin aglycone were less than 9.42%. All calibration curves showed good linearity (coefficient of determination = 0.99) within the tested ranges. The rapid and simultaneous u-HPLC method presented in this study significantly improved the speed, sensitivity and resolution of the analyses of nine types of anthocyanin glucosides and free delphidinin aglycone in grapes.

Rapid method for the simultaneous determination of flavonol aglycones in food using u-HPLC coupled with heating block acidic hydrolysis.

A rapid method for the simultaneous determination of flavonol aglycones in food using ultra-high-performance LC (u-HPLC) coupled with a heating-block acidic hydrolysis method was validated in terms of precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 micro m id, 2 mm, length 100 mm) with a photodiode array detector. The LOD and LOQ of the u-HPLC analyses were 0.15 and 0.47 mg/kg for myricetin, 0.09 and 0.28 mg/kg for quercetin, 0.16 and 0.49 mg/kg for kaempferol, and 0.08 and 0.25 mg/kg for isorhamnetin. The intraday and interday precisions of the individual flavonol aglycones were less than 9.31%. All calibration curves exhibited good linearity (r2 = 0.99) within the tested ranges. Total run time of u-HPLC was 13 min. The rapid u-HPLC method presented herein significantly improved the speed, sensitivity, and resolution of the analyses of myricetin, quercetin, kaempferol, and isorhamnetin in food.

Simultaneous determination of free capsorubin and capsanthin in red pepper powder using u-HPLC.

A simultaneous ultra-HPLC (u-HPLC) method for the determination of free capsorubin and capsanthin in red pepper powder was validated in terms of its precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 pm, id 2 mm length 100 mm) and with a photodiode-array detector. The recoveries of capsorubin were greater than 83.8 +/- 1.7%; the LOD and LOQ of the u-HPLC analyses were 0.043 and 0.129 mg/kg, respectively. The intraday and interday precisions for capsorubin were less than 9.01%. The recoveries of capsanthin were greater than 87.7 +/- 1.5%, and the LOD and LOQ were 0.101 and 0.306 mglkg, respectively. The intraday and interday precisions for capsanthin were less than 12.66%. All calibration curves for capsorubin and capsanthin exhibited good linearity (r2 = 0.99) within the tested ranges.

Determination of 22 ginsenosides in ginseng products using ultra-high-performance liquid chromatography.

A reverse-phase ultra-high-performance liquid chromatography (u-HPLC) method was developed for the rapid quantification of 22 ginsenosides in ginseng products. The proposed method for the analysis of ginsenosides is based on a heating-block method without further treatment. The u-HPLC separation was performed on a reversed C18 column (100 × 2 mm id, particle size 2 µm) followed by ultraviolet detection at 203 nm. Aqueous 50% methanol was used as the extraction solvent. The optimum amount of extraction solvent and the optimum extraction time were 20 mL and 20 min (extracted twice with 10 mL), respectively. The method validation parameters yielded good results for linearity, precision, accuracy and recovery. The recovery of ginsenosides from ginseng powder was greater than 98.1% and the limits of detection and quantification of the u-HPLC analysis were >0.6 and >1.8 mg/kg for ginsenosides. The calibration graphs for ginsenosides were linear from approximately 2.6 to 40.4 mg/kg for u-HPLC. The inter-day and intra-day precisions (relative standard deviation values) were <14.6 and 14.7%, except for Rg2(R) + Rh1(R).

Rapid method for the determination of vitamins A and E in foods using ultra-high-performance liquid chromatography.

A rapid and novel ultra-HPLC (u-HPLC) method for the determination of vitamins A (retinol) and E (alpha-, gamma-, and delta-tocopherol) in foods was validated in terms of its precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 microm, id 2 mm, and length 75 mm), followed by fluorescence detection. The recovery of retinol was more than 84.58%; the LOD and LOQ of the u-HPLC analysis were 0.015 and 0.045 mg/kg, respectively. The intraday and interday precision was less than 9.12%. The recoveries of alpha-, gamma-, and delta-tocopherol were more than 81.37%; the LOD and the LOQ were 0.014, 0.002, and 0.001 mg/kg and 0.042, 0.005, and 0.004 mg/kg, respectively. All calibration curves had good linearity (r2 = 0.99) within the test ranges. The novel, rapid method coupled to u-HPLC can provide significant improvements in the speed, sensitivity, and resolution compared with a conventional HPLC method.

Determination of hexanal as an oxidative marker in vegetable oils using an automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer.

An automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer was evaluated as an oxidative marker to determine hexanal content in vegetable oils. For the effective analysis, a cooled injection system (CIS) was used to focus and to introduce the hexanal desorbed from the Tenax TA. The temperature of the CIS was maintained at -60 °C for 12 min before desorbing the hexanal. Hexanal was separated on a capillary column (DB-5, 0.25 mm × 60 m, 0.25 µm in film thickness) from 50 to 230 °C, followed by mass spectrometer-selected ion monitoring analysis at m/z 56. The instrumental response to hexanal was highly linear from 10 ng mL(-1) to 1 µg mL(-1) (r(2) = 0.9999). The relative standard deviation (RSD) of intra- and inter-day repeatability was acceptable, with values of less than 3.88 and 4.25%, respectively. The LOD and LOQ of hexanal were determined by gas chromatograph/mass spectrometer-selected ion monitoring to be 3.3 and 9.8 ng mL(-1), respectively. The acid value, peroxide value and fatty acid composition revealed a good correlation with the hexanal concentration.

Rapid method for the determination of capsaicin and dihydrocapsaicin in Gochujang using ultra-high-performance liquid chromatography.

A sensitive and specific heating block method coupled with ultra-HPLC (u-HPLC) was developed for the analysis of capsaicin in Gochujang and validated by comparing with a conventional HPLC (AOAC Method 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The u-HPLC separation was performed on a reversed C18 column (50 x 2 mm id, particle size 2 microm), followed by fluorescence detection (excitation 280 nm, emission 325 nm). Methanol was used as the extracting solvent, and the amount of sample taken was approximately 0.2 g; the optimum amount of extraction solvent and extraction time were 15 mL and 1 h, respectively. The recovery of capsaicin in Gochujang was more than 93%, and the LOD and LOQ of the u-HPLC analysis were 0.05 and 0.16 microg/g for capsaicin and 0.05 and 0.16 microg/g for dihydrocapsaicin. The calibration graphs for capsaicin and dihydrocapsaicin were linear from 0.2 to 10.0 microg/mL for u-HPLC. The interday and intraday precisions (RSD values) were < 6.27%.