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目的建立高效液相色谱法(HPLC)测定佐匹克隆片有关物质含量的方法。方法采用C18柱,以含0.5%w/v十二烷基硫酸钠的0.01%w/v磷酸二氢钠溶液(用磷酸调节p H至4.0)—乙腈(62.5∶37.5)为流动相;检测波长为303 nm。结果佐匹克隆的检测限为2.4 ng,杂质2-氨基-5-氯吡啶的检测限为0.6 ng,定量限为2 ng;2-氨基-5-氯吡啶在0.1~10μg/ml浓度范围内线性关系良好,相关系数r=1.0000;各降解杂质与主药分离良好;低、中、高浓度下的平均加样回收率分别为103.41%、101.15%和100.95%,相对标准偏差为5.0%,回收率良好;供试品溶液在25℃环境中不稳定,需4℃保存进样。结论 HPLC方法灵敏度、准确度高,专属性强,可用于佐匹克隆片的有关物质检测。
Objective To establish a method for the determination of related substances in Zopiclone tablets by high performance liquid chromatography (HPLC). Methods A C18 column was used with a mobile phase of 0.01% w / v sodium dihydrogen phosphate (adjusted to pH to 4.0 with phosphoric acid) - acetonitrile (62.5: 37.5) containing 0.5% w / v sodium dodecyl sulfate. The wavelength is 303 nm. Results The detection limit of zopiclone was 2.4 ng, the detection limit of impurity 2-amino-5-chloropyridine was 0.6 ng, and the limit of quantification was 2 ng. The concentration of 2-amino-5-chloropyridine was in the range of 0.1-10 μg / The linear correlation was good with a correlation coefficient of r = 1.0000. The average separation recoveries were 103.41%, 101.15% and 100.95%, respectively. The relative standard deviations were 5.0% Good recovery; for the test solution instability in the environment of 25 ℃, 4 ℃ need to save the injection. Conclusion HPLC method has the advantages of high sensitivity, high specificity and strong specificity. It can be used to detect the related substances of zopiclone tablets.