• Asian-Australasian Journal of Animal Sciences
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• v.27 no.6
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• pp.871-879
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• 2014

Two experiments were conducted to determine the digestible energy (DE) and metabolizable energy (ME) contents of corn gluten feed (CGF) for finishing pigs and to develop equations predicting the DE and ME content from the chemical composition of the CGF samples, as well as validate the accuracy of the prediction equations. In Exp. 1, ten CGF samples from seven provinces of China were collected and fed to 66 finishing barrows (Duroc${\times}$Landrace${\times}$Yorkshire) with an initial body weight (BW) of $51.9{\pm}5.5$ kg. The pigs were assigned to 11 diets comprising one basal diet and 10 CGF test diets with six pigs fed each diet. The basal diet contained corn (76%), dehulled soybean meal (21%) and premix (3%). The ten test diets were formulated by substituting 25% of the corn and dehulled soybean meal with CGF and contained corn (57%), dehulled soybean meal (15.75%), CGF (24.25%) and premix (3%). In Exp. 2, two additional CGF sources were collected as validation samples to test the accuracy of the prediction equations. In this experiment, 18 barrows (Duroc${\times}$Landrace${\times}$Yorkshire) with an initial BW of $61.1{\pm}4.0$ kg were randomly allotted to be fed either the basal diet or two CGF containing diets which had a similar composition as used in Exp. 1. The DE and ME of CGF ranged from 10.37 to 12.85 MJ/kg of dry matter (DM) and 9.53 to 12.49 MJ/kg of DM, respectively. Through stepwise regression analysis, several prediction equations of DE and ME were generated. The best fit equations were: DE, MJ/kg of DM = 18.30-0.13 neutral detergent fiber-0.22 ether extract, with $R^2$ = 0.95, residual standard deviation (RSD) = 0.21 and p<0.01; and ME, MJ/kg of DM = 12.82+0.11 Starch-0.26 acid detergent fiber, with $R^2$ = 0.94, RSD = 0.20 and p<0.01. These results indicate that the DE and ME content of CGF varied substantially but the DE and ME for finishing pigs can be accurately predicted from equations based on nutritional analysis.

• Korean Journal of Food Science and Technology
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• v.52 no.6
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• pp.580-586
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• 2020

Fishery resources have been widely consumed as protein- and vitamin-rich food sources in the Korean diet. However, information regarding their vitamin levels is extremely limited. In this study, trienzyme-Lactobacillus casei method was validated and used to determine the folate contents in fishery foods. The trienzyme-L. casei method for folate analysis showed excellent accuracy (85.2 to 95.3% recovery) and precision (repeatability 1.4% RSD and reproducibility 2.4% RSD). Folate contents of 20 fish foods (4 fish, 3 crustaceans, 3 sea algae, 3 cephalopods, 4 shellfish, and 3 others) ranged from 1.75 to 97.98 ㎍/100 g. Furthermore, we found that the folate content in seaweed fusiforme was the highest, followed by gulfweed (69.73 ㎍/100 g). Folate analysis using the trienzyme-L. casei method was determined excellent based on the z-score of -0.3 in the Food Analysis Performance Assessment Scheme test. Analytical and method validation data generated in this study could be used to update the national food composition table on vitamin B9 in Korean fishery resources.

• Korean Journal of Environmental Agriculture
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• v.29 no.2
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• pp.165-175
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• 2010

A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

• Analytical Science and Technology
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• v.30 no.6
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• pp.379-389
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• 2017

In this study, we set up an analytical method that can be used for rapid and accurate determination of representative isoquinoline alkaloids in medicinal plants using UPLC-ESI-Q-TOF MS (ultra pressure liquid chromatography-electrospray ionization-quadrupole-time-of-flight mass spectrometry). The compounds were eluted on a C18 column with 0.1 % formic acid and acetonitrile, and separated with good resolution within 13 min. Each of the separated components was characterized by precursor ions (generated by ESI-Q-TOF) and fragment ions (produced by collision-induced dissociation, CID), which were used as a reliable database. We also performed method validation: analytes showed excellent linearity ($R^2$, 0.9971-0.9996), LOD (5-25 ng/mL), LOQ (17-82 ng/mL), accuracy (91.6-97.4 %) as well as intra- and inter-day precisions (RSD, 1.8-3.2 %). In the analysis of Chelidonium majus L., magnoflorine, coptisine, sanguinarine, berberine and palmatine were detected by matching retention times and characteristic fragment ion patterns of reference standards. We also confirmed that, among the quantified components, coptisine was present in the highest quantity. Furthermore, alkaloid profiling was carried out by analyzing the fragment ion patterns corresponding to peaks of unknown components. In this manner, protopine, chelidonine, stylopine, dihydroberberine, canadine, and nitidine were tentatively identified. We also proposed the molecular structure of the fragment ions that appear in the mass spectrum. Therefore, we concluded that our suggested method for the determination of major isoquinoline alkaloids by UPLC-Q-TOF can be useful not only for quality control, but also for rapid and accurate investigation of phytochemical constituents of medicinal plants.

• Natural Product Sciences
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• v.17 no.2
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• pp.147-159
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• 2011

A high-performance liquid chromatography-electrospray ionization-tandem mass spectrometric method was developed to determine simultaneously eight marker constituents of Forsythiae fructus, and subsequently applied it to classify its two botanical origins. The marker compounds of Forsythia suspensa were phillyrin, pinoresinol, phillygenin, lariciresinol and forsythiaside; those of F.viridissima were arctiin, arctigenin and matairesinol. Separation of the eight analytes was achieved on a phenyl-hexyl column (150${\times}$2.0 mm i.d., 3 ${\mu}M$) using gradient elution with the mobile phase: (A) 10% acetonitrile in 0.5% acetic acid, (B) 40% aqueous acetonitrile. A few fragment ions specific to the types of lignans, among the product ions generated by collisonally induced dissociation (CID) of molecular ion clusters, such as [M-H]$^-$ or [M+OAc]$^-$ were used not only for fingerprinting analysis but for the quantification of each epimer by using multiple-reaction monitoring mode. It was shown good linearity ($r^2{\geq}$ 0.9998) over the wide range of all analytes; intra- and inter-day precisions (RSD, %) were within 9.14% and the accuracy ranged from 84.3 to 115.1%. The analytical results of 40 drug samples, combined with multivariate statistical analyses - principal component analysis (PCA) and hierarchical cluster analysis (HCA) - clearly demonstrated the classification of the test samples according to their botanical origins. This method would provide a practical strategy for assessing the authenticity or quality of the herbal drug.

• Toxicological Research
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• v.31 no.3
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• pp.255-264
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• 2015

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.