CAJ | 학술논문

建立HPLC-MS-MS法测定比格犬血浆中盐酸戊乙奎醚浓度的方法.盐酸戊乙奎醚血浆样品经石油醚-乙醚(7:3)混合溶液萃取后进样.色谱柱为Agilent反相XDB-C18柱(4,6 mm×150 mm, 5 μm),流动相为甲醇-5 mmol/L醋酸铵水溶液(90:10,v/v,pH 5.8).采用电喷雾离子源,正离子模式,MRM离子采集方式,采集离子(m/z)盐酸戊乙奎醚316.4-128.2[M+H]+,内标盐酸苯海拉明256.4-167.2[M+H]+.标准曲线在1 ng/mL-1000 ng/mL范围内呈线性,相关系数为0.9988.定量下限为0.05 ng/mL.方法的精密度、准确度和回收率均符合要求.分别给予静脉注射0.5,1和5 mg/kg剂量PH后,主要的药动学参数如下:t1/2α0.33 h,t1/2β 2.44 h,tmax 0.058 h,AUC和Cmax与剂量呈线性递增.三个剂量组均符合二室模型.此方法测定比格犬血浆中盐酸戊乙奎醚浓度灵敏、准确、快速,适用于常规盐酸戊乙奎醚药动学研究.
건립HPLC-MS-MS법측정비격견혈장중염산무을규미농도적방법.염산무을규미혈장양품경석유미-을미(7:3)혼합용액췌취후진양.색보주위Agilent반상XDB-C18주(4,6 mm×150 mm, 5 μm),류동상위갑순-5 mmol/L작산안수용액(90:10,v/v,pH 5.8).채용전분무리자원,정리자모식,MRM리자채집방식,채집리자(m/z)염산무을규미316.4-128.2[M+H]+,내표염산분해랍명256.4-167.2[M+H]+.표준곡선재1 ng/mL-1000 ng/mL범위내정선성,상관계수위0.9988.정량하한위0.05 ng/mL.방법적정밀도、준학도화회수솔균부합요구.분별급여정맥주사0.5,1화5 mg/kg제량PH후,주요적약동학삼수여하:t1/2α0.33 h,t1/2β 2.44 h,tmax 0.058 h,AUC화Cmax여제량정선성체증.삼개제량조균부합이실모형.차방법측정비격견혈장중염산무을규미농도령민、준학、쾌속,괄용우상규염산무을규미약동학연구.
To develop a fast and sensitive liquid chromatography-mass spectrometry method for the determination of penehyclidine hydrochloride (PH) in beagle dog plasma. PH and diphenhydramine hydrochloride (internal standard, IS) were extracted with a solvent mixture of petroleum ether-ethyl ether (7:3). Chromatographic separation was achieved on a reversed-phase Eclipse XDB-C18 column (4.6 mm×l50 ram, 5 μm) using the eluent of methanol-water (5 mmol/L ammonium acetate) (90:10, v/v, pH 5.8) as mobile phase. The electrospray ionization source was set at the positive multiple reaction monitoring (MRM) mode. This method involved the use of the [M+H]+ions of PH and diphenhydramine hydrochloride at m/z 316.4-128.2 and m/z 256.4-167.2. The calibration curve was linear in the range of 1-1000 ng/mL with a correlation coefficient of 0.9988. The lower limit of quantification was 0.05 ng/mL. The precision, accu- racy and recovery of the method were acceptable. Following intravenous injection administration at doses of 0.5, 1 and 5 mg/kg PH, the main pharmacokinetic paraneters were as the followings, t1/2α 0.33 h, t1/2β 2.44 h,tmax 0.058 h, AUC and Cmax exhibited a linear increase along with the increase of dose. The two-compartment model fit the three dose groups. This method was sensitive, accurate and fast for the determination of concentration of PH in beagle dog plasma. It could be used in pharmacokinetic studies of PH.