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[摘要]
目的 建立氢溴酸替格列汀中遗传毒性杂质溴乙烷残留量的气相色谱(GC)检测方法。方法 采用迪马DM-624色谱柱(30 m×0.53 mm×3.0 μm);电子捕获检测器(ECD);程序升温:初始柱温40 ℃,保持3 min,以20 ℃/min升温至200 ℃,保持5 min;进样口温度:210 ℃;检测器温度:210 ℃;载气:氮气;分流比:3:1;进样量1 μL。结果 溴乙烷在0.75~6.75 μg/mL与峰面积呈良好的线性关系(r=0.999 7),最低检测限为0.26 μg/mL。平均回收率为99.4%,RSD值为0.3%(n=9)。3批氢溴酸替格列汀样品中均未检测出溴乙烷。结论 该方法简便、准确,重复性好,适用于氢溴酸替格列汀中溴乙烷残留量的控制。
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[Abstract]
Objective To establish a gas chromatography (GC) method for the determination of bromoethane residues in teneligliptin hydrobromide. Methods The determination was carried out on Dikma DM-624 chromatographic column (30 m × 0.53 mm, 3.0 μm) with ECD detector. The column temperature was raised from 40 ℃ (kept for 3 min) to 200 ℃ (then kept for 5 min) by program at the rate of 20 ℃/min. The injector temperature was 210 ℃, and the detector temperature was 210 ℃. Nitrogen was used as carrier gas. The injection volume was 1 μL with 3∶1 as split ratio. Results The linearity range of bromoethane was 0.75 — 6.75 μg/mL (r = 0.999 7). The minimum detectable limit was 0.26 μg/mL. The average recovery was 99.4% with RSD value of 0.3% (n = 9). Bromoethanes in three batches of teneligliptin hydrobromide samples were not detected. Conclusion The method is sample, accurate, reproducible, and applicable to the residues control of bromoethane in teneligliptin hydrobromide.
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