Lei Shuo, Gao Xun, Sun Yang, Yu Xiangyong, Zhao Longshan
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China.
Liaoning Medical Device Test Institute, Shenyang 110179, China.
J Pharm Anal. 2018 Dec;8(6):373-377. doi: 10.1016/j.jpha.2018.06.003. Epub 2018 Jun 26.
A simple method was established for the determination of -propiolactone (BPL) in human inactivated rabies vaccine by gas chromatography-mass spectrometry (GC-MS). The determination was performed on an Agilent HP-INNOWAX (30 m × 0.32 mm i.d., 0.25 µm) capillary column at the temperature of 80 °C. Electrospray ionization (ESI) was used by selective ion detection at 42. The temperature for ESI source and inlet was set at 230 °C and 200 °C, respectively. Helium was used as the carrier gas at a flow rate of 25.1 mL/min. The total run time was 8 min. Acetonitrile and other components in the sample did not interfere with the determination of BPL. The results showed good linearity of BPL in the range of 0.50-10.01 μg/mL, with the limit of detection and the limit of quantification of 0.015 μg/mL and 0.050 μg/mL, respectively. Satisfactory precision was achieved for the current developed method. The method was applied to detect 6 batches of vaccine samples, and the results indicated that the target analyte BPL was present in three batches of unpurified samples, but was not detected in the purified samples, indicating the test samples were qualified. The established method was proved to be simple, versatile and sensitive, which can meet the requirements of quality control of BPL in human inactivated rabies vaccine.
建立了一种采用气相色谱 - 质谱联用（GC - MS）测定人用狂犬病灭活疫苗中β - 丙内酯（BPL）的简单方法。测定在安捷伦HP - INNOWAX（30 m×0.32 mm内径，0.25 µm）毛细管柱上进行，柱温为80℃。采用电喷雾电离（ESI），在m/z 42处进行选择性离子检测。ESI源温度和进样口温度分别设置为230℃和200℃。以氦气作为载气，流速为25.1 mL/min。总运行时间为8分钟。样品中的乙腈和其他成分不干扰BPL的测定。结果表明，BPL在0.50 - 10.01 μg/mL范围内具有良好的线性关系，检测限和定量限分别为0.015 μg/mL和0.050 μg/mL。所建立的方法具有令人满意的精密度。该方法应用于检测6批疫苗样品，结果表明目标分析物BPL存在于3批未纯化样品中，但在纯化样品中未检测到，表明测试样品合格。所建立的方法被证明简单、通用且灵敏，能够满足人用狂犬病灭活疫苗中BPL质量控制的要求。
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