• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.18 no.1
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• pp.40-46
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• 2013

The isotope ratios of $^{13}C/^{12}C$ and $^{18}O/^{16}O$ for a sample in a mass spectrometer are measured relative to those of a pure $CO_2$ reference gas (i.e., laboratory working standard). Thus, the calibration of a laboratory working standard gas to the international isotope scales (Pee Dee Belemnite (PDB) for ${\delta}^{13}C$ and Vienna Standard Mean Ocean Water (V-SMOW) for ${\delta}^{18}O$) is essential for comparisons between data sets obtained by other groups on other mass spectrometers. However, one often finds difficulties in getting well-calibrated standard gases, because of their production time and high price. Additional difficulty is that fractionation processes can occur inside the gas cylinder most likely due to pressure drop in long-term use. Therefore, studies on laboratory production of pure $CO_2$ isotope standard gas from stable solid calcium carbonate standard materials, have been performed. For this study, we propose a method to extract pure $CO_2$ gas without isotope fractionation from a solid calcium carbonate material. The method is similar to that suggested by Coplen et al., (1983), but is better optimized particularly to make a large amount of pure $CO_2$ gas from calcium carbonate material. The $CaCO_3$ releases $CO_2$ in reaction with 100% pure phosphoric acid at $25^{\circ}C$ in a custom designed, evacuated reaction vessel. Here we introduce optimal procedure, reaction conditions, and samples/reactants size for calcium carbonate-phosphoric acid reaction and also provide the details for extracting, purifying and collecting $CO_2$ gas out of the reaction vessel. The measurements for ${\delta}^{18}O$ and ${\delta}^{13}C$ of $CO_2$ were performed at Seoul National University using a stable isotope ratio mass spectrometer (VG Isotech, SIRA Series II) operated in dual-inlet mode. The entire analysis precisions for ${\delta}^{18}O$ and ${\delta}^{13}C$ were evaluated based on the standard deviations of multiple measurements on 15 separate samples of purified $CO_2$. The pure $CO_2$ samples were taken from 100-mg aliquots of a solid calcium carbonate (Solenhofen-ori $CaCO_3$) during 8-day experimental period. The multiple measurements yielded the $1{\sigma}$ precisions of ${\pm}0.01$‰ for ${\delta}^{13}C$ and ${\pm}0.05$‰ for ${\delta}^{18}O$, comparable to the internal instrumental precisions of SIRA. Therefore, we conclude the method proposed in this study can serve as a way to produce an accurate secondary and/or laboratory $CO_2$ standard gas. We hope this study helps resolve difficulties in placing a laboratory working standard onto the international isotope scales and does make accurate comparisons with other data sets from other groups.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.20 no.1
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• pp.41-51
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• 1987

This study was carried out to prepare powdered smoked-dried mackerel which can be used as a soup base, and to examine storage stability and the taste compounds of Products. Raw mackerel are filleted, toiled for 10 minutes and pressed to remove lipids, and then soaked in extract solution of skipjack meat. This soaked mackerel are smoked 3 times to $10-12\%$ moisture content at $80^{\circ}C$ for 8 hours. And the smoked-dried mackerel were pulverized to 50 mesh. Finally, the powdered smoked-dried mackerel were packed in a laminated film $bag(PET/Al\;foil/CPP:\;5{\mu}m/15{\mu}m/70{\mu}m,\;15\times17cm)$ with air(product C), nitrogen(product N) and oxygen absorber(product O), and then stored at room temperature for 100 days. The moisture and crude lipid content of powdered smoked-dried mackerel was $11.3-12.3\%,\;12\%$, respectively, and water activity is 0.52-0.56. And these values showed little changes during storage. The pH, VBN and amino nitrogen content increased slowly during storage. Hydrophilic and lipophilic brown pigment formation showed a tendency of increase in product(C) and showed little change in product(N) and (O). The TBA value, peroxide value and carbonyl value of product(N) and (O) were lower than those of product (C). The major fatty acids of products were 16:0, 18:1, 22:6, 18:0 and 20:5, and polyenoic acids decreased, while saturated and monoenoic acids increased during processing and storage of products. The IMP content in products were 420.2-454.2 mg/100 g and decreased slightly with storage period. And major non-volatile organic acids in products were lactic acid, succinic acid and $\alpha-ketoglutaric$ acid. In free amino acids and related compounds, major ones are histidine, alanine, hydroxyproline, lysine, glutamic acid and anserine, which occupied $80.8\%$ of total free amino acids. The taste compounds of powdered smoked-dried mackerel were free amino acids and related compounds (1,279.4 mg/100 g), non-volatile organic acids(948.1 mg/100 g), nucleotides and their related compounds (672.8 mg/100 g), total creatinine(430.4 ntg/100 g), tetaine(86.6 mg/100 g) and small amount of TMAO. The extraction condition of powdered smoked-dried mackerel in preparing soup stock is appropriate at $100^{\circ}C$ for 1 minute. Judging from the results of taste and sensory evaluation, it is concluded that the powdered smoked-dried mackerel can be used as natural flavoring substance in preparing soups and broth.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.