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.
Analytical method for synephrine and octopamine in citrus fruits, drinks containing citrus fruit, and human urine was developed using gas chromatography / mass spectrometry(GC/MS). Silylation with MSTFA, acetylation with MBTFA, and trimethylailylation with MSTFA followed by tritluoroacetylation with MBTFA were compared. The selective derivatization of aynephrine and octopamine was optimized with two derivatizing reagents ; MSTFA and MBTFA. The ion at mlz 267 was monitored to characterize the benzyl group of the both compounds. Synephrine was detected in the concentrations of 0.46-1.88 ug/g for citrus fruits and 1.2-8.1 ug/ml for drinks. The urinary excretion data of aynephrine showed the highest concentration at the period of 8-20 hours after drinking orange juices and total amounts of its urinary excretion calculated as a parent compound was 11-14% of a dose during 48 hours. Octopamine was not detected in citrus fruits, drinks, and human urine.
H대학 실습선 28명의 선원에 대하여 40일간 장기간 항해 전과 후의 혈액과 소변의 생화학적 분석을 실시하였다. 원앙 후 부원 및 모든 연령에서 요소질소와 요산수치(creatine 및 uric acid)가 증가된 것으로 보아 선상생활이 신장의 기능을 나쁘게 하거나 기능저하를 초래했다고 판단되어진다. 또 총콜레스테롤(TC)과 고밀도지단백콜레스테롤(HDL-C) 및 저밀도지단백콜레스테롤(LDL-C)은 원양 전보다 후에 유의하게 감소한 반면에 중성지방(TG)은 유의하게 상승하였다. 연령별로는 TC와 HDL-C가 30대, 40대에서 유의하게 감소하였고, TG는 30대가 유의하게 증가하였는데 특히 30대에서 몇몇 선원에 대해서는 원양 후 TG의 높은 증가를 보여 고지혈증이 의심되고 있다. 또한 소변검사에서도 간세포성기능 및 신장기능의 이상을 진단하는 담즙색소(UBG)와 요단백(PRO)에서 장기간 항해 전과 후 모두 양성반응이 나타난 선원이 각각 7명과 5명 이었다. 특히 우로빌리노겐(Urobilinogen : UBG)에서 양성반응이 크게 증가하여 한 달간 원앙을 통하여 간세포성기능이 저하되었거나 이상이 있음을 보여주고 있다.
생쥐에서 페르몬으로 알려진 소수성의 분자와 결합하는 major urinary proteins(MUPs)는 부분적으로 성장 호르몬(GH)의 조절을 받는다. 본 연구에서는 MT-GRF로 형질전환되어 성장호르몬이 증가된 생쥐에서 MUP의 발현을 조사하였다. 이 MT-GRF로 형질전환된 생쥐의 소변에서 MUP이 대조군보다 심하게 저하되어 나타났고, 암컷보다 수컷에서 더 저하되어 나타났다. 또한 MT-GRF를 근육에 주사한 생쥐에서도 MUP는 저하되어 나타났다.