摘要
目的建立高效液相色谱法同时测定对乙酰氨基酚口服混悬液中有关物质及防腐剂.方法采用高效液相色谱法.色谱柱为Hypersil GOLD C18色谱柱,流动相A为0.1%三氟乙酸溶液,流动相B为0.1%三氟乙酸的乙腈溶液,梯度洗脱,流速为每分钟1.0ml,柱温35℃,检测波长为245nm,进样量20μl.结果有关物质杂质A(对乙酰氨基酚二聚体)、杂质B(对氯乙酰苯胺)以及7个未知杂质,防腐剂苯甲酸、对羟基苯甲酸丁酯均能与主成分及各种辅料完全分离;杂质A、杂质B以及防腐剂苯甲酸、对羟基苯甲酸丁酯的检测质量浓度分别在0.016μg/ml~6.4μg/ml、0.032μg/ml~0.384μg/ml、0.85μg/ml~16.95μg/ml、0.125μg/ml~2.4μg/ml范围内与各自峰面积积分值呈良好的线性关系(r=1、1、0.9999、1),检测限分别为0.065ng、0.14ng、0.34ng、0.10ng,定量限分别为0.32ng、0.67ng、1.71ng、0.26ng,平均回收率分别为99.0%、95.4%、99.8%、100.0%.结论该方法灵敏、准确、专属性强、重复性好,可用于对乙酰胺基酚口服混悬液的质量控制.
Objective To establish a HPLC method for the simultaneous determination of related substances and preservatives in paracetamol oral suspension.Methods HPLC method was adpotted.The determination was performed on Hypersil gold C18 column,mobile phase A was 0.1%trifluoroacetic acid solution,mobile phase B was 0.1%trifluoroacetic acid in acetonitrile,gradient elution,flow rate was 1.0ml per minute,column temperature was 35℃,detection wavelength was 245n m,and injection volume was 20μl.Results The elated substances impurity A(Acetaminophen dimer),impurity B(P-chloroacetanilide),a nd seven unknown impurities,the preservatives benzoic acid,butylparahen could be completely separated from the principal components as well as various excipients;The detection concentration of impurity a,impurity B,preservative benzoic acid and butylparahen showed a good linear relationship with their respective peak area integral values in the range of 0.016μg/ml~6.4μg/ml(r=1),0.032μg/ml〜0.384μg/ml(r=1),0.85μg/ml~16.95μg/ml(r=0.9999)and 0.125μg/ml〜2.4μg/ml(r=l),The limits of detection were 0.065 ng,0.14 ng,0.34 ng,0.10 ng,and the limits of quantification were 0.32ng,0.67ng,1.71ng,0.26ng.The average recover was 99.0%,95.4%,99.8%,100.0%.Conclusions The developed method is sensitive,accurate,specific and reproducible and can be applied to the quality control of oral suspensions of acetaminophen.
作者
范保瑞
张悦
张成志
王正中
Fan Baorui;Zhang Yue;Zhang Chengzhi;Wang Zhengzhong(Beijing Pinggu District food and drug safety monitoring center,Beijing 101200;Shanghai Johnson Pharmaceutical Co.,Ltd,Shanghai 200245)
出处
《首都食品与医药》
2021年第8期176-180,共5页
Capital Food Medicine
基金
国家药典委员会质量标准提高,国药典综发[2013]349号。
