目的 建立氫溴酸替格列汀中遺傳毒性雜質(zhì)溴乙烷殘留量的氣相色譜（GC）檢測方法。方法 采用迪馬DM-624色譜柱（30 m×0.53 mm×3.0 μm）；電子捕獲檢測器（ECD）；程序升溫：初始柱溫40 ℃，保持3 min，以20 ℃/min升溫至200 ℃，保持5 min；進樣口溫度：210 ℃；檢測器溫度：210 ℃；載氣：氮氣；分流比：3：1；進樣量1 μL。結(jié)果 溴乙烷在0.75～6.75 μg/mL與峰面積呈良好的線性關(guān)系（r=0.999 7），最低檢測限為0.26 μg/mL。平均回收率為99.4%，RSD值為0.3%（n=9）。3批氫溴酸替格列汀樣品中均未檢測出溴乙烷。結(jié)論 該方法簡便、準確，重復(fù)性好，適用于氫溴酸替格列汀中溴乙烷殘留量的控制。

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.