反相离子对色谱法同时测定工业品硝唑尼特中硝唑尼特及其代谢物脱乙酰基-硝唑尼特  

Simultaneous Determination of Industrial Grade Nitazoxanide and its Metabolite Desacetyl Nitazoxanide by Reversed Phase Ion Pair Chromatography

作　　者：吴清盛[1] 茅小燕[1] 罗妮娜[1] 李峰[1] 

机构地区：[1]浙江育英职业技术学院,浙江杭州310018

出　　处：《化学试剂》2014年第4期340-342,共3页Chemical Reagents

摘　　要：应用0．015moL／L正己烷磺酸钠为离子对试剂，V（0．015mol／LKH2PO．（pH2．5）水溶液）：V（乙腈）=65：35为流动相，在ZobaxEclipseXDBC8色谱上，采用外标法，建立了工业品硝唑尼特中硝唑尼特及其代谢物脱乙酰基-硝唑尼特的反相离子对高效液相色谱分析方法，硝唑尼特的相对标准偏差〈0．2％，脱乙酰基-硝唑尼特的相对标准偏差〈1％。样品进样量在0．4—4μg范围内硝唑尼特r=0．9999，脱乙酰基-硝唑尼特r=0．9999。硝唑尼特检测限为0．5μg／mL，脱乙酰基．硝唑尼特检出限为0．05μg,／mL。应用0．015mol／L正己烷磺酸钠为离子对试剂，以外标法建立了工业品硝唑尼特及其代谢物脱乙酰基．硝唑尼特的反相离子对高效液相色谱分析方法，色谱条件为：流动相为y（0．015mol／LKH2PO4（pH2．5）水溶液）：V（乙腈）=65：35，色谱柱为ZobaxEclipseXDBC8色谱柱，流速为1．0mL／min，检测波长为360nm。结果显示，该方法在样品进样量为0．4—4μg范围内硝唑尼特和脱乙酰基-硝唑尼特相对标准偏差分别〈0．2％和1％，相关系数都为r=0．9999，硝唑尼特和脱乙酰基-硝唑尼特检测限分别为0．5μg／mL和0．05μg／mL。This work proposed a method using reversed phase ion pair chromatography for simuhaneous determination of in- dustrial grade nitazoxanide and its metabolite desacetyl nita- zoxanide. The instrument used was Agilent HPLC with a Zob- ax Eclipse XDB C8 column. 0.015 mol/L hexane sulfonic acid sodium and 0.015 moL/L KH2PO＋ （ pH 2.5 ）/acetoni- trile＇water solution （ V/V 65/35） was separately used as ion pair reagent and the mobile phase. The flow rate was 1.0 mL/ min, and the detection wave was 360 rim. The calibration curve was linear （ r = 0. 999 9） within the range of 0. 4 - 4 μg for nitazoxanide and desacetyl nitazoxanide. The relative deviation of nitazoxanide and desacetyl nitazoxanide was less than 0.2% and 1% ,respectively. The detection limit for nita- zoxanide and desacetyl nitazoxanide was 0. 5 μg/mL and 0.05 p.g/mL,respectively.

关 键 词：唑尼特 脱乙酰基-硝唑尼特 反相离子对色谱法 

分 类 号：O657.7[理学—分析化学]