RP-HPLC法测定药用胶塞中16种多环芳烃含量并作模拟提取研究

Determination of 16 Polycyclic Aromatic Hydrocarbons in Pharmaceutical Rubber Plugs by RP-HPLC and Thier Migration

目的:本试验通过高效液相色谱法测定药用胶塞中16种多环芳烃(PAHs)的含量并作迁移试验。方法:色谱柱为Kromasil 100-5-C18(4.6 mm×250 mm,5μm);以乙腈和水为流动相,采用梯度洗脱进行分离:0~27 min,乙腈-水(65∶35);27~41 min,乙腈-水(65∶35)→(100∶0);41~43 min,乙腈-水(100∶0)→(65∶35);43~55 min,乙腈-水(65∶35)。检测波长:220、254、295 nm。结果:16种PAHs在0.1000~10.00μg·mL-1浓度范围内线性关系良好,均r≥0.999;定量限在2.505~83.20 ng·mL^-1;检测限在0.7515~24.96 ng·mL^-1;精密度RSD均≤2.0%;重复性RSD≤3.0%;平均加样回收率为88.74%~99.27%。试验同时考察16种多环芳烃(PAHs)的迁移试验,以验证该方法。结论:试验采用的RP-HPLC法测定16种PAHs方法专属性良好,能够快捷、简便、准确、灵敏地测定药用胶塞中16种PAHs的含量,可适用于橡胶胶塞中PAHs的测定以及考察注射液中16种PAHs的迁移。

Objective: To establish a HPLC method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in rubber plugs and to test their migration. Methods: A Kromasil 100-5-C18 (4.6 mm × 250 mm, 5 μm) column under gradient elution was used for separation;PAHs from the rubber plugs were extracted through ultrasonics and the analysis was tested for linearity, LOD, LQD, precision, repeatability and recovery. Results: A good linear relationship were obtained when the concentrations of the 16 PAHs were within the ranges, with the correlative coefficient r>0.999;LQD were at 2.505-83.20 ng·mL^-1;LOD were at 0.751 5-24.96 ng·mL^-1;RSD for precision were less than 2.0%, repeatability RSD were less than 3.0%;The average recovery were at 88.74%-99.27%. The migration of the 16 PAHs were tested to verify the specificity of the method. Conclusion: In this study, the method established is rapid, simple, accurate and reliable for the determination of PAHs in the rubber plugs and their migration in injections to ensure drug safety.