CAJ | 학술논문

目的：建立超高效液相色谱－串联质谱（ UPLC－MS／MS）法测定血浆中尼洛替尼浓度方法。方法以卡马西平为内标，用蛋白沉淀前处理方法。色谱柱为 ACQUITY UPLC BEH C18（100 mm ×2．1 mm，1．7μm），流动相为乙腈－0．1％甲酸水溶液（35∶65），流速为0．4 mL? min －1，正离子模式多反应监测（ MRM）扫描分析，并考察专属性、标准曲线与定量下限、精密度与回收率、基质效应和稳定性。结果血浆中尼洛替尼线性范围为0．1～20．0μg? mL －1（ r ＝0．998），定量下限为0．1μg? mL －1，提取回收率在95．11％～101．32％，日内、日间精密度相对标准偏差（ RSD）均小于15％。结论该法操作简便快速，特异性强，灵敏度高，可用于尼洛替尼的治疗药物浓度监测。
목적：건립초고효액상색보－천련질보（ UPLC－MS／MS）법측정혈장중니락체니농도방법。방법이잡마서평위내표，용단백침정전처리방법。색보주위 ACQUITY UPLC BEH C18（100 mm ×2．1 mm，1．7μm），류동상위을정－0．1％갑산수용액（35∶65），류속위0．4 mL? min －1，정리자모식다반응감측（ MRM）소묘분석，병고찰전속성、표준곡선여정량하한、정밀도여회수솔、기질효응화은정성。결과혈장중니락체니선성범위위0．1～20．0μg? mL －1（ r ＝0．998），정량하한위0．1μg? mL －1，제취회수솔재95．11％～101．32％，일내、일간정밀도상대표준편차（ RSD）균소우15％。결론해법조작간편쾌속，특이성강，령민도고，가용우니락체니적치료약물농도감측。
Objective To establish a UPLC-MS/MS method for the determination of nilotinib in human plasma.Methods The plasma procedure involved a single-step protein precipitation by acetonitrile, then separation was carried out using a ACQUITY UPLC BEH C18 column ( 100 mm ×2.1 mm, 1.7 μm) with a mobile phase consisted of acetonitrile -0.1% formic acid ( 35∶65 ) at a flow rate of 0.4 mL? min -1 .The protonated ions of analytes were detected in positive ionization by multiple reaction monitoring mode ( MRM ) .The speci-ficity, standard curve, lower limit of quantitation, precision, recovery rate and stability as well as the matrix effect were investigated. Results The calibration curve was linear over a concentration range of 0.1 to 20.0 μg? mL -1 ( r=0.998) and the low limit of quantita-tion was 0.1 μg? mL -1 .The extraction recovery rates were ranged from 95.11% to 101.32%, with-day RSD and between-day RSD were all less than 15%.Conclusion The method is simple and quick, with high specificity and sensitivity, and suitable for clinical therapeutic drug monitoring of nilotinib.