响应面结合柱前衍生-HPLC法测定盐酸达泊西汀中甲醛含量  

Determination of formaldehyde in dapoxetine hydrochloride by response surface methodology combined with pre-column derivatization-HPLC

作　　者：唐莲 杨仁明 TANG Lian;YANG Renming(Chengdu DIAO Pharmaceutical Group Co.,Ltd.,Chengdu,Sichuan 610041,China;Sichuan Aupone GOOD Pharmaceutical Co.,Ltd.,Chengdu,Sichuan 610097,China)

机构地区：[1]成都地奥制药集团有限公司,四川成都610041 [2]四川奥邦古得药业有限公司,四川成都610097

出　　处：《安徽医药》2025年第5期914-919,共6页Anhui Medical and Pharmaceutical Journal

摘　　要：目的建立盐酸达泊西汀中甲醛含量检测的高效液相色谱(HPLC)方法,以期为盐酸达泊西汀中甲醛的控制提供参考。方法采用中心组合-响应面法(CCD-RSM)对甲醛的衍生条件进行优化后,结合HPLC法对甲醛含量进行测定,用十八烷基键合硅胶为填充剂(Gemini C_(18),4.6 mm×250 mm,5μm);以乙腈-水(60∶40,v/v)为流动相,等度洗脱;检测波长为354 nm;流速为每分钟1.0 mL;柱温为40℃;进样体积20μL。结果采用CCD-RSM优化后的衍生条件为:衍生温度为35℃,衍生时间为40 min,衍生剂比例为20∶1;线性方程为Y=727194X+625.91;相关系数r=0.9998;定量限为0.004 mg/L;平均加标回收率为97.86%,相对标准差(RSD)(n=9)为2.12%。结论该法专属性强、重复性好和准确度高,可用于盐酸达泊西汀中甲醛的控制。Objective To establish an HPLC method for the detection formalde hyde in dapoxetine hydrochloride.Methods The central combination design-response surface method(CCD-RSM)was used to optimize the derivation conditions of formaldehyde,and the formaldehyde content was determined by HPLC.The column was Gemini C_(18)(4.6 mm×250 mm,5μm);the mobile phase was acetonitrile∶water=60∶40,isometric elution;the detection wavelength was 354 nm;the flow rate was 1.0 mL/min;the column temperature was 40℃;the injection volume was 20μL.Results The derivatization conditions optimized by CCD-RSM were as follows:the derivatization temperature was 35℃,the derivatization time was 40 min,and the ratio of derivatizing agents was 20∶1;the linear equation was Y=727194X+625.91;r=0.9998;the LOQ was 0.004 mg/L;the average recovery rate was 97.86%,and the RSD(n=9)was 2.12%.Conclusions The method has strong specificity,good repeatability,accurate and reliable results,and can be used for the control of formaldehyde in dapoxetine hydrochloride.

关 键 词：达泊西汀 药物污染 甲醛 响应面 柱前衍生 高效液相色谱 遗传毒性杂质 含量 

分 类 号：R927[医药卫生—药学] R927.2