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

• Journal of Korean Society of Forest Science
• /
• v.16 no.1
• /
• pp.1-32
• /
• 1972

By means of the interspecific hybridization in the Sub-genus Diploxylon of the Genus Pinus, $F_1$ hybrids of Pinus rigida${\times}$elliottii, Pinus rigida${\times}$radiata, P. rigida${\times}$serotina and P. densiflora${\times}$thunbergii had been produced. And on the basis of the crossabilities of these hybrids the taxonomic affinities of these pines were examined. And the needle characteristics of these hybrid and the occurence of phenolic substances in these $F_1$ hybrid were also investigated to see the potential usefulness of these characteristics for the diagnosis of the taxonomic affinity. And, the growth performances of the $F_1$ hybrids have also been compared with those of parental species. In order to contribute to the establishment of the hybrid seed orchard the introgression phenomena between P. densiflora and P. thunbergii in the eastern coastal area have also been investigated along with the investigation of the heterozygosity of plus trees of P. densiflora growing in the clone bank in Suwon. And the results were summarized as follows. 1. On the basis of crossabilities as well as on the taxonomic affinities according to the systems of Shaw, Pilger and Duffield, it has been proven that the parental species of those hybrids are of close affinities and range of the fertile hybrid seed production rate was as high as 28-58% in the best hybrid combination (Table 13). 2. Among those hybrids, the ${\times}$ Pinus, rigiserotina hybrid seemed to be most promising in the growth performance exhibiting 109-155% more volume growth compared to the seed parent with the statistic significance of 1% level (Tables 16 and 17). 3. Notwithstanding the fact that the all of the pollen parents are cold tender, all hybrids exhibit cold hardiness as much as their seed parent and it seems to suggest that the characteristics of cold hardiness were transmitted from the seed parent. 4. Though a striking difference in needle length was observed between the parental species of each hybrid, it was difficult to distinguish each hybrid from their seed parent by the needle length except ${\times}$P. rigiserotina which is characterized by long needle which is 65% more longer than the needle of the seed parent (Table 21). 5. With regard to the anatomical characteristics of needle, the hypoderm is apparently thicker in most of the $F_1$ hybrid pines and the characteristics of resin canals are dominated by medial in most $F_1$ hybrid. And, the fibrovascular bundles were apart as were in their seed parent. Therefore it was found to be possible to distinguish the hybrids pines from their parents by the needle characteristics. And, it is to be noticed that the ${\times}$P. densithunbergii was more close to the pollen parent having RDI value of 0.73 (Fig.l, Table 22). 6. It has been demonstrated that ${\times}$P. rigielliottii, ${\times}$P. rigiradiata and ${\times}$P. rigitaeda have a phenolic substance (No.7) of light yellow at Rf-0.46, same as their seed parent, but no trace of phenolic substance was observed in their pollen parent. This fact will serve as an important criteria for early identification of hybridity in progeny testing. However, the fact that both of ${\times}$P. rigiserotina and ${\times}$P. densithunbergii exhibit the same reactions of phenolic substances as well their parental species seems to indicate the close affinities between the parental species of the respective hybrid (Fig.2, Table 23). 7. The separation and the reaction of phenolic substance developed on TLC were found to be same in the same species showing no variations between the individuals, and no variations due to tree part of sampling, tree age or pollen sources. And the reaction was also observed regardless of the not varied by the kind of developing solvent whether it is Aceton-Chloroform (3:7 v/v) or Benzene-Methanol-Acetic acid (90:16:8 v/v). 8. The introgression phenomena of natural Pinus densifiora stand in both east and west coastal area indicates that the major part of the red pines investigated are all heterozygous and the heterozygosity of pines are higher in the west coast than in the east coast(Tables 24 and 25). 9. Based on the RDI, among the plus trees of Pinus densiflora selected in Korea and Japan as well, no pure P. densiflora has been found. Since all of the sample trees of Pinus densiflora were found to be as heterozygous bearing part of the characteristics of P. thunbergii, those red pines were considered to be natural heterotic hybrid pines(Figs. 3 and 4. Tables 26 and 27).