The Animal and Plant Quarantine Agency conducts a targeted sampling plan and analysis for veterinary drugs within the country every year. Target compounds included tetrachlorvinphos as an organophosphate, diminazene as an anti-infective medication, ketoprofen as a nonsteroidal anti-inflammatory drug, triclabendazole and clorsulon as flukicides in 2022. These compounds were not included in National Residues Program (NRP), despite their high sales ranking. A total of 94 bovine muscle samples and 20 equine muscle samples were collected from various locations across the country. The analysis of target compounds in muscle was performed using LC-MS/MS coupled with Food code 8.3.1 revised in 2022. A 2 g sample of muscle tissue was extracted using a water: acetonitrile (1:4, v/v) solution, then cleaned up with C18 and hexane saturated with acetonitrile. Compounds were separated with C18 column and mobile phases consisted of 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B). All analytes exhibited good linearity with correlation coefficients (R2) higher than 0.992. The limit of quantification (LOQ) of these compounds ranged from 0.21 to 2.79 μg/kg except for diminazene (3.85~6.86 μg/kg). The average recoveries of these analytes were 89.45~129.13% in muscle at spiked level of 10 or 20 μg/kg. Relative standard deviations (%) (intra-day and inter-day) were lower than 20% for all target compounds, except for diminazene and triclabendazole, whose intra-day RSD % was slightly higher than 20% in equine muscle. Testing confirmed that all 94 bovine and 20 equine muscle samples from 9 provinces were free from residues of veterinary drugs. Monitoring of compounds not included in the NRP should continue to ensure consumer health and food safety.
This study aims to establish a modified analytical method with sensitivity and reliability for streptomycin (STP) and dihydrostreptomycin (DHS) of residues level in pig tissues, plasma and urine by LC-MS/MS on the basis of previous studies. The mass parameters of quantitative and qualitative ions for STP and DHS were optimized using multiple reaction monitoring in positive mode. The separation of compounds was conducted using BEH Amide column according to material’s characteristics. The analytes in plasma were extracted with only organic solvents. In muscle and kidney, KH2PO4 buffer solution containing 2% CCl3COOH and EDTA-Na was used as extraction solvent. The WCX cartridege was selected as SPE cartridge in considering high recoveries for STP and DHS. The analytes in urine were extracted by organic solvents with acid and addition of EDTA. The limits of detection (LODs) in STP and DHS ranged 0.45~3.66 μg/kg and 0.22~0.78 μg/kg, respectively. The limits of quantification (LOQs) were 1.35~11.10 μg/kg in STP and 0.66~2.36 μg/kg in DHS. The recoveries (%) were 94.29~104.5% in STP and 92.32~108.45% in DHS except for plasma with lower values (61.45/68.5%, respectively). In the precision evaluation, the coefficient of variation (CV, %) of STP showed <10.50% on intra-day and <18.04% on inter-day. The CV (%) of DHS showed <8.42% on intra-day, whereas <17.98% on inter-day. The modified method is reliable for continuous residual monitoring in pig to ensure food safety for consumer’s health. In addition, this method could be used in study relation to residue depletion and pharmacokinetics of veterinary drug.
본 연구는 참당귀 재배 시에 발생하는 추대 참당귀를 부산물로 활용가능성이 있는지 평가하기 위해 수행하였다. 추대 참당귀의 지상부와 지하부의 총 무게는 수확기 비추대 참당귀의 지하부 무게 대비 약 98.5%로 높게 나타났다. 또한 추대 당귀의 decursin과 decursinol angelate의 총 함량은 주 생산품인 참당귀 신(身)의 지표성분 총 함량인 4.24%와 대비해 부위별로 0.64%~2.39%로 나타났으며, 이는 추출물로 이용 시 생산품 대비 15~56%에 해당하는 것으로 나타났다. 또한, 항상화 활성의 경우 추대 참당귀는 전반적으로 비추대 참당귀에 비해 우수한 것으로 나타났다. 추대 참당귀의 생산량, 지표성분 함량 그리고 항산화 활성 결과를 고려해 봤을 때, 추대 참당귀의 부산물은 사료 첨가제 및 화장품 용도의 추출물로 이용 가능성이 높은 것으로 생각된다.
Angelica gigas Nakai (AGN) is a traditional medicinal herb especially in Korea. It contains pyranocoumarins, which are major active components including decursin (D) and decursinol angelate (DA). This study was carried out to determine the change in active component content and antioxidant activity depending on the root diameter of AGN. Several processing steps are involved to use AGN roots as medicine. The dried AGN roots are divided into body (B), thick root (TkR), medium root (MR) and thin root (TnR) according to their diameter before cutting into medicine. The recovery rates of each root parts per 100 ㎏ were measured as 32.3±2.5, 9.0±1.0, 39.3±2.1 and 15.0±1.0%, respectively and the mean diameters were measured as 51.95±4.55, 7.05±0.89, 2.88±0.49 and 1.57±0.32 ㎜. Two index components, D and DA, were analyzed. The change of both D and DA content showed a similar tendency. Both D and DA content were increased as the root diameter decreased (higher in TnR). In addition, antioxidant activity was higher in B and TnR, and lower in TkR and MR than control. This study showed that the thinner the root diameter, the higher the D and DA content in AGN roots and that TnR has excellent antioxidant activity compared to other root parts, suggesting that the thinner root part of AGN could be used as a potential material.