CAJ | 학술논문

建立反相高效液相色谱辅-光电二极管阵列检测器( RP-HPLC)法同时测定丁酸氯维地平原料药中的10种杂质。色谱柱为 Symmetry C18柱(250 mm×4.6 mm,5μm),流动相为0.05 mol/L NaH2PO4溶液(pH 2.5)-乙腈/甲醇(3：2, V/V),梯度洗脱,柱温35℃,流速为1.5 mL/min,检测波长220 nm。丁酸氯维地平及其10个已知杂质能够达到良好的分离,且各组分在各自测定浓度范围内与峰面积的线性关系良好(r≥0.9970)；丁酸氯维地平及杂质1~10的检出限(S/N=3)在0.15~0.90 mg/L之间。本方法快速、简便、有效,可用于丁酸氯维地平原料药的质量控制管理。
건립반상고효액상색보보-광전이겁관진렬검측기( RP-HPLC)법동시측정정산록유지평원료약중적10충잡질。색보주위 Symmetry C18주(250 mm×4.6 mm,5μm),류동상위0.05 mol/L NaH2PO4용액(pH 2.5)-을정/갑순(3：2, V/V),제도세탈,주온35℃,류속위1.5 mL/min,검측파장220 nm。정산록유지평급기10개이지잡질능구체도량호적분리,차각조분재각자측정농도범위내여봉면적적선성관계량호(r≥0.9970)；정산록유지평급잡질1~10적검출한(S/N=3)재0.15~0.90 mg/L지간。본방법쾌속、간편、유효,가용우정산록유지평원료약적질량공제관리。
A reversed phase high performance liquid chromatographic ( RP-HPLC) method coupled with DAD was developed for the simultaneous determination of ten process-related impurities ( PRI ) of Clevidipin Butyrate ( CLE). The chromatographic separation was carried out on a Waters symmetry C18 column (250 mm ×4. 6 mm, 5 μm) and all components were monitored at 220 nm. The mobile phase consisted of 0. 05 mol/L sodium dihydrogen phosphate with pH 2. 5 adjusted by phosphoric acid ( MPA ) and a mixed solution of acetonitrile and methanol (3:2, V/V). Flow rate was kept at 1. 5 mL/min, the injection volume was 20 μL for all injections, and the column temperature maintained at 35 ℃. The method was further validated with respect to selectivity, linearity, limit of detection ( LOD ), limit of quantitation ( LOQ ), precision and accuracy. A good linearity was obtained in the measured concentration ranges for CLE and ten impurities ( r≥0. 9970 ), and the detection limits were 0. 90, 0. 24, 0. 23, 0. 15, 0. 18, 0. 18, 0. 27, 0. 82, 0. 45, 0. 89 and 0. 45 mg/L for CLE and ten impurities respectively.