目的：建立苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定方法及指纹图谱质量控制方法。方法采用气相色谱法和液相色谱法分别建立苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定方法及指纹图谱质量控制方法。气相色谱法中样品采用甲醇回流法提取,选择萘为内标物,建立方法学。液相色谱法中样品采用乙酸乙酯提取,300 nm为检测波长,甲醇-0.1%甲酸水梯度洗脱,建立指纹图谱质量控制方法。结果气相色谱法中薄荷脑和龙脑的线性范围分别为0.312~0.0156 mg·mL-1(r=0.9999),0.2016~0.01008 mg·mL-1(r=0.9999)；平均加样回收率分别为100.99%(RSD=3.97%, n=6),97.61%(RSD=2.09%,n=6),薄荷脑、龙脑的精密度、重复性及稳定性的RSD均小于3%,所检测的20批次苍耳子鼻炎滴丸样品中薄荷脑和龙脑含量范围分别为1.34%~2.29%,1.15%~1.61%。在色谱指纹图谱中,共确定了19个共有峰,利用对照品对共有峰中的3个最高色谱峰进行了指认,采用该方法测定20批次样品,除2个批次外,其余样品相似度均在0.95以上。结论所建立的含量测定及指纹图谱质量控制方法准确、可靠,可有效地用于苍耳子鼻炎滴丸的质量控制。%Objective To establish a method of gas chromatography and the HPLC fingerprint to evaluate the quality of Cangerzi rhinitis drop pills.Methods Using the internal standard method to analyze the content of menthol and borneol in rhinitis dripping pills by gas chromatography. Samples were extracted using methanol and the methodology was established. Ethyl acetate was applied in extracting HPLC ifngerprint sample. The detected wave length was 300 nm. The separation was performed with a gradient elution composed of methanol and 0.1% formic acid-water.Results The linear range of menthol was 0.312~0.015 6 mg·mL-1, r=0.999 9, the average recovery was 100.99% (RSD=3.97%, n=6). The linear range of borneol was 0.201 6~0.010 08 mg·mL-1, r=0.999 9, the average recovery rate was 97.61% (RSD=2.09%, n=6). The RSD of precision, repeatability and stability in two components were less than 3%. The concentration of menthol and borneol in Cangerzi rhinitis dropping pills was within the range of 1.34%~2.29% and 1.15%~1.61%, respectively. In the ifngerprint, 19 characteristic peaks were established, and three of that were identiifed. Twenty batches of Cangerzi rhinitis drop pills were determined and the similarities of 18 batches were above 0.95.Conclusion Results show that the method of gas chromatography and ifngerprint is convenient,accurate and reliable,which can be applied to control the quality of Cangerzi rhinitis dripping pills.
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