GC-MS法测定复方肝浸膏制剂中棕榈酸和硬脂酸

目的：建立气质联用法测定复方肝浸膏制剂中棕榈酸和硬脂酸。方法：用甲醇超声提取复方肝浸膏片（胶囊）中的棕榈酸和硬脂酸，经气相色谱分离后，用质谱对化学成分进行确认，标准曲线法计算含量。色谱条件：HP-5MS毛细管柱（30 m×0.25 mm，0.25 μm）；程序升温，进样口温度250℃，载气为高纯氦气（1.0 mL·min^-1）；质谱条件：电离方式为EI，电离能量70 eV，离子源温度230℃，棕榈酸定量离子和定性离子分别为m/z 73.0和60.0、73.0、129.1、213.2，硬脂酸定量离子和定性离子分别为m/z 73.0和73.0、129.1、185.1、241.2。结果：棕榈酸和硬脂酸质量浓度分别在6.45~1 032 μg·mL^-1和6.65~1 064 μg·mL^-1内线性良好（r=0.999），棕榈酸和硬脂酸的平均回收率（n=9）为101.5和102.8%；不同厂家19批片剂中棕榈酸和硬脂酸的含量分别为1.2~7.8和1.3~9.5 mg·片^-1，4批胶囊剂中棕榈酸和硬脂酸的含量分别为4.0~6.3和3.4~7.8 mg·粒^-1。结论：经方法学验证，本方法可用于复方肝浸膏片（胶囊）中棕榈酸和硬脂酸的测定。

Objective: To establish a GC-MS analysis method for the contents determination of palmitic acid and stearic acid in compound Hepar Extractum preparations. Methods: The samples were extracted by ultrasonic wave, and separated using gas chromatography. The stearic acid and palmitic acid were confirmed by GC-MS and quantitatively analyzed with standard curve method. Chromatographic conditions:an HP-5MS capillary column (30 m×0.25 mm,0.25 μm) was used with column temperature raised by programming,the injector temperature was 250℃, and the carrier gas was helium(1.0 mL·min^-1). MS conditions:the ionization mode was EI, the electron energy was 70 eV,the ion source temperature was 230℃. The quantitative and qualitative ions were m/z 73.0 and 60.0, 73.0, 129.1, 213.2 for palmitic acid, and m/z 73.0 and 73.0, 129.1, 185.1, 241.2 for stearic acid were monitored. Results: The linearity ranges of palmitic acid and searic acid were 6.45-1 032 μg·mL^-1(r=0.999) and 6.65-1 064 μg·mL^-1(r=0.999), respectively; the average recoveries(n=9) were 101.5% and 102.8%, respectively. 19 batches of tablets and 4 batches of capsules from different manufacturers were determined, the contents of palmitic acid and stearic acid in tablets were 1.2-7.8 and 1.3-9.5 mg per tablet,and the two compounds in capsules were 4.0-6.3 and 3.4-7.8 mg per capsule, respectively. Conclusion: The established method is proved by methodology validation that it can be used for the determination of palmitic acid and stearic acid in compound Hepar Extractum tablets(capsules).

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