摘要
目的建立高效液相色谱(HPLC)法同时测定复方樟脑乳膏中樟脑和水杨酸甲酯含量的方法,并与气相色谱(GC)法比较。方法 HPLC法采用Alltima C18(150 mm×4.6 mm,5μm)色谱柱,紫外检测器,乙腈-10%甲醇水(50∶50)为流动相,流速为0.8 mL·min^-1,樟脑和水杨酸甲酯的检测波长分别为287 nm和304 nm。GC法采用Rtx-wax色谱柱(30 m×0.25 mm,0.25μm),FID检测器,柱温为120℃,保持20 min,萘为内标。结果 HPLC法中樟脑和水杨酸甲酯分别在0.202~2.0175mg·mL^-1和0.025 24~0.8076 mg·mL^-1与相对应色谱峰峰面积线性关系良好;GC法中樟脑和水杨酸甲酯分别在0.5038~3.779 mg·mL^-1和0.3929~2.947 mg·m L^-1与其峰面积与内标峰面积的比值线性关系良好。水杨酸甲酯和樟脑的平均回收率分别为98.7%~99.3%,99.1%~99.5%(HPLC法);100.1%~100.7%,99.4%~100.6%(GC法);RSD值均<2.0%(n=3)。样品测定结果进行统计分析,差异无统计学意义。结论 HPLC法与GC法均可以用于复方樟脑乳膏中樟脑和水杨酸甲酯的含量测定,GC法略优于HPLC法,但HPLC法更适合医疗机构中含樟脑和水杨酸甲酯成分制剂的质量控制。
Objective To establish an HPLC method for the content determination of camphor and methylsalicylate in compound camphor cream, and compared it with GC method. Methods The HPLC separation was performed on an Alltima C18 (150 mm×4.6 mm, 5 μm) column with 10% menthol solution-acetonitrile (50 ∶ 50, v/v) as the mobile phase. The UV detection was at 287 nm for camphor and 304 nm for methyl salicylate, respectively. The flow rate was 0.8 mL·min^-1 . Chromatography conditions of GC method included Rtx-WAX capillary column (30 m×0.25 mm, 0.25 μm) and FID detector. The column temperature was 120℃, which was kept for 20 min. Naphthalene was used as the internal standard. Results The linear ranges of camphor and methylsalicylate with HPLC method were 0.202 - 2.0175 mg·mL^-1 and 0.025 24 - 0.8076 mg·mL^-1 , respectively. While the linear ranges of camphor and methyl salicylate with GC method were 0.5038 - 3.779 mg·mL^-1 and 0.3929 - 2.947 mg·mL^-1 , respectively. The average recoveries of methylsalicylate and camphor determined were 98.7%-99.3% and 99.1%-99.5% by HPLC, and 100.1%-100.7% and 99.4%-100.6% by GC. The RSD values were all less than 2.0%(n = 3), with no significant difference (P > 0.05). Conclusion HPLC and GC in the determination of camphor and methylsalicylate vary. HPLC is better suited for the quality control of the hospital preparations.
作者
何笑荣
张闪闪
谭湘珊
邝咏梅
金鹏飞
HE Xiao-rong;ZHANG Shan-shan;TAN Xiang-shan;KUANG Yong-mei;JIN Peng-fei(Department of Pharmacy,Beijing Hospital,National Center of Gerontology,Beijing 100730;Aerospace Gentral Hospital,Beijing 100039)
出处
《中南药学》
CAS
2019年第6期872-875,共4页
Central South Pharmacy
