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目的:建立测定莪术油聚氰基丙烯酸正丁酯毫微粒(ZTO-PBCA-NP)中莪术油的主要成分β-榄香烯、莪术酮、莪术醇和莪术二酮含量的气相色谱-质谱方法。方法:采用HP-5MS毛细管色谱柱(30.0 m×250μm×0.25μm),进样温度250℃,不分流;程序升温:初始65℃恒温2 min,以5℃.min-1升至90℃恒温3 min,以20℃.min-1升至103℃恒温3 min,以8℃.min-1升至150℃恒温15 min,以20℃.min-1升至280℃。结果:β-榄香烯、莪术酮、莪术醇和莪术二酮进样浓度在4.00～40.00μg.mL-1范围内与峰面积呈良好线性关系(r=0.9979～0.9997);平均回收率(n=4)分别为98.3%(RSD=2.8%),99.4%(RSD=2.1%),95.5%(RSD=1.6%),101.2%(RSD=2.5%)。结论:该方法专属性强,准确度高,重复性好,可用于ZTO-PBCA-NP的质量控制。
OBJECTIVE: To establish a gas chromatography-mass spectrometry (GC-MS) method for the determination of β-elemene, curcumol, curcumol and zedrone in the essential oil of ZTO-PBCA-NP. Methods: HP-5MS capillary column (30.0 m × 250 μm × 0.25 μm) was used. The injection temperature was 250 ℃ and splitless. The program temperature was raised to 65 ℃ for 2 min, and then to 5 ℃ .min- 3 min to 20 ℃ .min-1 to 103 ℃ constant temperature for 3 min, 8 ℃. Min-1 to 150 ℃ constant temperature 15 min, 20 ℃. Min-1 rose to 280 ℃. Results: The calibration curves of β-elemene, curcumol, curcumol and zedrone were linear with the peak area in the range of 4.00-40.00 μg.mL-1 (r = 0.9979-0.9997). The average recovery (n = 4) were 98.3% (RSD = 2.8%), 99.4% (RSD = 2.1%), 95.5% (RSD = 1.6%) and 101.2% (RSD = 2.5%), respectively. Conclusion: This method is highly specific, accurate and repeatable and can be used for quality control of ZTO-PBCA-NP.