| 唐莲,杨仁明.响应面结合柱前衍生 -HPLC法测定盐酸达泊西汀中甲醛含量[J].安徽医药,2025,29(5):914-919. |
| 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 |
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| DOI：10.3969/j.issn.1009-6469.2025.05.012 |
| 中文关键词: 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 |
| 英文关键词: Dapoxetine Drug contamination Formaldehyde Response surface methodology Pre-column derivatization HPLC Genotoxic impurity Determination |
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| 摘要点击次数: 50 |
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| 中文摘要: |
| 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 C18，4.6 mm×250 mm，5 μm)；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 20 μL。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=727 194X+625.91；相关系数 r=0.999 8；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。 |
| 英文摘要: |
| 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, andthe formaldehyde content was determined by HPLC. The column was Gemini C18 (4.6 mm×250 mm, 5 μm); the mobile phase was aceto-nitrile∶water=60∶40, isometric elution; the detection wavelength was 354 nm; the flow rate was 1.0 mL/min;the column temperaturewas 40 ℃ ; the injection volume was 20 μL.Results The derivatization conditions optimized by CCD-RSM were as follows: the de-rivatization temperature was 35 ℃, the derivatization time was 40 min, and the ratio of derivatizing agents was 20∶1; the linear equa-tion was Y=727 194X+625.91; r=0.999 8; 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 con-trol of formaldehyde in dapoxetine hydrochloride. |
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