高效液相色谱法测定清洁验证中残留物盐酸帕罗西汀的含量

Determination of paroxetine hydrochloride residues in cleaning validation by HPLC

目的建立清洁验证中残留物盐酸帕罗西汀含量测定的高效液相色谱法。方法色谱柱为phenomenex Kinetex C18(4.6 mm×75 mm,2.6μm),流动相为醋酸铵水溶液(取醋酸铵3.85 g,加水600 mL使溶解,加三乙胺10 mL,用冰醋酸调节pH值至5.5)-乙腈(65∶35),流速1.0 mL·min^-1,检测波长295 nm,进样体积30μL,柱温25℃。结果帕罗西汀在0.1~25μg·m L^-1与峰面积线性关系良好,加样回收率为101.9%~108.1%,擦拭取样回收率为74.8%和81.1%。结论该方法专属性好、精密度和准确度高,可用于清洁验证中盐酸帕罗西汀残留物的快速定量分析。

Objective To determine paroxetine hydrochloride residues in the cleaning validation by HPLC. Methods HPLC was conducted on a phenomenex Kinetex C18 column(4.6 mm×75 mm, 2.6 μm) with a mixture of ammonium acetate solution(3.85 g of ammonium acetate in 600 mL of water, adding 10 mL of trimethylamine and adjusting to pH 5.5 with acetic acid)-acetonitrile(65 ∶ 35) as the mobile phase. The flow rate was 1.0 mL·min^-1, the detection wavelength was 295 nm, the injection volume was 30 μL, and the column temperature was 25 ℃. Results The standard curve of paroxetine showed a good linearity at 0.1 to 25 μg·mL^-1. The sample recovery was 101.9%-108.1%. The extraction recoveries were 74.8% and 81.1%. Conclusion This method is suitable for the rapid quantitative determination of paroxetine hydrochloride residues in the cleaning validation with good specificity, precision and accuracy.