HPLC法测定劳拉西泮片有关物质的含量

摘要

目的：建立劳拉西泮片的含量及有关物质的HPLC方法。方法以十八烷基硅烷键合硅胶作为填充剂的ZORBAX SB－C18柱（250 mm ×4．6 mm，5μm）为色谱柱，流动相：0．05 mol·L－1的磷酸二氢铵（含0．5％的三乙胺，用磷酸调pH至2．5）∶甲醇∶乙腈＝35∶35∶30；流速：1．0 mL·min－1；检测波长：235 nm；进样量：10μL；柱温：30℃。结果劳拉西泮峰及各杂质峰均能良好分离。杂质A浓度与峰面积在1．5μg·L－1～8．048 mg·L－1内线性关系良好。杂质B浓度与峰面积在15．0μg·L－1～8．224 mg·L－1内线性关系良好。杂质C浓度与峰面积在1．7μg·L－1～8．144 mg·L－1内线性关系良好；杂质D浓度与峰面积在2．5μg·L－1～8．032 mg·L－1内线性关系良好；杂质E浓度与峰面积在3．0μg·L－1～8．032 mg·L－1内线性关系良好。测定样品含量平均值为97．9％，有关物质均符合要求。结论该方法快速、简单，稳定，重现性好，可作为劳拉西泮片的含量及有关物质的检测方法。%Objective To determine the related substances and content in iorazepam tablets by HPLC.Methods The chromatographic separation was performed on ZORBAX SB-C18 column (4.6 mm ×250 mm,5 μm)that was made by alkyl-bonded silica gels.The mobile phase was 0.05 mol·L-1 ammonium dihydrogen orthophosphate (including 0.5%trimethylamine and pH adjusted to 2.5 with phosphoric acid)∶methanol∶acetonitrile=35∶35∶30.The flow rate was 1 .0 mL·min-1 ,the detection wavelength was 235 nm,the sam-ple size was 10 μL,and the column temperature was set at 30℃.Results The resolution between iorazepam and the other peaks met the requirements.The linearity ofrelated substance A concentration and peak area was 1.5 μg·L-1 ~8.048 mg·L-1.The linearity of related substance B concentration and peak area was 15.0 μg·L-1 ~8.224 mg·L-1 .The linearity of related substance C concentra-tionandpeakareawas1.7 μg·L-1 ~8.144mg·L-1.ThelinearityofrelatedsubstanceDconcentrationandpeakareawas2.5 μg· L-1 ~7.952 mg·L-1 .The linearity of related substance E concentration and peak area was 3.0 μg·L-1 ~8.032 mg·L-1 .Determi-nation of the sample average content was 97.9%,and the related substance met the requirements.Conclusions The method was quick,simple,stable,and well repeatable,which could be used to determine the content of iorazepam tablets and its related substances.