目的 采用氣相色譜-電子捕獲檢測器（GC-ECD）法測定奧美沙坦酯原料藥中基因毒性雜質(zhì)碘甲烷。方法 采用Agilent DB-624毛細(xì)管色譜柱（30 m×0.32 mm×1.8 μm），初始柱溫40℃，保持5 min，以20℃/min升至200℃，保持2 min，進(jìn)樣口溫度160℃，檢測器溫度300℃，載氣為N₂，體積流量為1.5 mL/min，分流比10：1，進(jìn)樣量1 μL。結(jié)果 碘甲烷在0.03~0.60 μg/mL線性關(guān)系良好；檢測限為2.0 ng/mL，定量限為6.0 ng/mL；平均回收率為98.0%，RSD值為1.8%。結(jié)論 該方法專屬性強(qiáng)、準(zhǔn)確性高、靈敏度高、耐用性好，可用于奧美沙坦酯中基因毒性雜質(zhì)碘甲烷的測定。

Objective To determine the genotoxic impurity methyl iodide in olmesartan medoxomil API by GC-ECD method. Methods The genotoxic impurity was detected on a Agilent DB-624 capillary column (30 m×0.32 mm×1.8 μm). The column temperature was programmed:the initial temperature was 40℃ and was maintained for 5 min. Then the temperature was raised to 200℃ at a rate of 20℃/min and maintained for 2 min. The inlet temperature was 160℃, and electron capture detector temperature was 300℃. N₂ was used as the carrier gas, and the flow rate was 1.5 mL/min, the split ratio was 10:1, the injection volume was 1 μL. Results At the range of 0.03-0.60 μg/mL, the regression equation of methyl iodide was good. The LOD concentration was 2.0 ng/mL, and the LOQ concentration was 6.0 ng/mL. The average recovery rate was 98.0% with the RSD value was 1.8%. Conclusion This method is high specificity, accuracy, sensitivity, and well durability, which can be used for the detection of the genotoxic impurity methyl iodide in olmesartan medoxomil API.

R927.2