目的 建立注射用益氣復脈（凍干）（YQFM）中氯化丁基橡膠塞用棕櫚酸和硬脂酸的含量測定方法，并對其穩(wěn)定性進行考察。方法 采用HP-5MS （30 mm×0.25 mm，0.25 μm）氣相色譜柱，柱溫程序為初始溫度150℃，5℃/min升至190℃保持2 min，5℃/min升至240℃保持10 min，體積流量1.8 mL/min，進樣口250℃，檢測器250℃，分流比1.0。進行專屬性、線性關系、加樣回收率、精密度、穩(wěn)定性、耐用性方法學考察。選取6批YQFM（對應2個廠家的膠塞）倒立放置于下述環(huán)境進行試驗，加速條件：溫度（40±2）℃、相對濕度（75±5）%，長期條件：溫度（25±2）℃、相對濕度（60±5）%，分別對0時，加速1、2、3、6個月及長期3、6、9、12、18、24、36個月各6批制劑中棕櫚酸和硬脂酸含量進行測定。結果 棕櫚酸和硬脂酸專屬性良好，在各自濃度范圍內(nèi)線性關系良好（r>0.999），檢出限和定量限分別為0.1 μg/mL和1.0 μg/mL，加樣回收率分別為93.92%、106.20%，穩(wěn)定性、精密度及耐用性結果均符合要求。在加速及長期試驗中，6批YQFM中棕櫚酸和硬脂酸的含量與0時相比基本相當或略有增加，沒有明顯的變化，均遠小于限度值。結論 所建立的GC法準確可靠，可用于YQFM中棕櫚酸和硬脂酸的含量測定；藥品隨著時間放置，棕櫚酸和硬脂酸含量遠低于安全限值，對產(chǎn)品質量不會造成安全風險。

Objective To establish a method for the content determination of palmitic acid and stearic acid in butyl rubber plug of YiqiFumai Lyophilized Injection and to investigate the stability ofsamples. Methods Using HP-5MS (30 mm×0.25 mm, 0.25 μm) gas chromatography column, the column initial temperature was 150℃, 5℃/min rose to 190℃ for two min, then 5℃/min rose to 240℃ for 10 min, the volume flow rate was 1.8 mL/min, the inlet temperature was 250℃, the detector temperature was 250℃and the split ratio was 1.0. Results The linear relationship of palmitic acid and stearic acid were good in their own ranges (r>0.999). The average recovery of palmitic acid and stearic acid was 93.32% and 106.20% respectively. The precision and durability results are in line with the requirements; the content of palmitic acid and stearic acid in the study on the stability of YiqiFumai Lyophilized Injection sample was below the limit. Specificity, linear relationship, sample recovery, precision, stability and durability were investigated. Six batches of YQFM (corresponding to rubber plugs from two manufacturers) were selected and placed upside down in the following environment for test. Acceleration conditions were temperature (40 ±2)℃, relative humidity (75 ±5)%, and longterm conditions were temperature (25 ±2)℃ and relative humidity (60 ±5)%. The contents of palmitic acid and stearic acid in 6 batches of preparation at 0, 1, 2, 3, 6 months of acceleration conditions and 3, 6, 9, 12, 18, 24, 36 months of long-term conditions were determined respectively. Conclusion The established method was accurate and reliable and can be used for the determination of palmitic acid and stearic acid in YiqiFumai Lyophilized injection. The content of palmitic acid and stearic acid is far below the safety limit as the drug is placed over time, which does not pose a safety risk to the product quality.

R284.1