冷柱头气相色谱法测定示踪剂18FPBR06注射液中有机溶剂含量

Determination of Organic Solvent in Radioactive Tracer 18FPBR06 Injection by Cold-on-Column Inlet Gas Chromatography

  • 摘要: 为了推动神经炎症正电子发射断层显像示踪剂18FPBR06的应用,本研究开发了一种能够同时测量18FPBR06注射液中乙醇含量和残留溶剂质量控制检验方法。采用Stabilwax色谱柱(30 m×0.52 mm,1 μm),程序升温:初始温度55 ℃,保持4 min,再以40 ℃/min升温至200 ℃,保持3 min。氢火焰离子化检测器温度240 ℃,载气为高纯氮气,进样口压力5.5 psi(37.9 kPa)。冷柱头进样口温度跟随柱温。结果显示,乙醇、乙腈、DMSO分别在0.5%~12.0%(v·v-1),0.004 0%~ 0.048 0%(g·g-1)和0.025%~0.590%(g·g-1)范围内具有良好线性关系,定量限(S/N=10)分别为0.15%(v·v-1),0.002 9%(g·g-1)和0.008 2%(g·g-1);检测限(S/N=3)分别为0.05%(v·v-1),0.000 87%(g·g-1)和0.002 5%(g·g-1)。加标回收率考察表明,该方法具有良好的准确度。方法学验证结果表明,本研究开发的冷柱头进样口直接进样GC法满足《中国药典》2020年版的相关要求,适用于18FPBR06注射液中乙醇和残留溶剂含量检查,并具有样品量少、稳定性好、快速的优点,能够提高产品质控检查效率。

     

    Abstract: To develop a quality control inspection method for determining content of ethanol and residual solvent in radiolabeled tracer 18FPBR06 injection which is used for positron emission tomography imaging. Stabilwax CG column (30 m×0.52 mm, 1 μm) is selected. Temperature program: set initial temperature at 55 ℃, kept for 4 min, then increased to 200 ℃ at rate of 40 ℃/min, hold for 3 min. Hydrogen flame ionization detector is used and the temperature is 240 ℃. The carrier gas is high-purity nitrogen, and the inlet pressure is 5.5 psi (37.9 kPa). The temperature of Cold-on-Column inlet follows the column temperature. The results show that ethanol, acetonitrile, and DMSO have good linear relationships in the concentration range of 0.5%-12.0% (v·v-1), 0.004 0%-0.048 0% (g·g-1) and 0.025%-0.590% (g·g-1). The limit of quantification (S/N=10) for ethanol, acetonitrile, and DMSO is 0.15% (v·v-1), 0.002 9% (g·g-1) and 0.008 2% (g·g-1). The limits of detection (S/N=3) is 0.05% (v·v-1), 0.000 87% (g·g-1) and 0.002 5% (g·g-1), respectively. The results of the standard addition recovery show that the method has good accuracy. The Cold-on-Column inlet GC method developed in this study is suitable for inspecting the content of ethanol, acetonitrile and DMSO in 18FPBR06 injection. The results of the method validation meet the requirements of the Chinese Pharmacopoeia 2020 edition. The method is accurate and time-saving, requiring only a small volume of sample, which is beneficial to improve the efficiency of product quality control inspection.

     

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