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目的:建立一种新的、稳定的微乳体系,并应用微乳液相色谱法同时测定白术药材中白术内酯Ⅰ、Ⅲ的含量。方法:考察影响分离的主要因素:表面活性剂、助表面活性剂、油相、p H、温度、色谱柱等,得到微乳体系为3.3%(w/v)十二烷基硫酸钠-8.25%(v/v)正丁醇~(-1).15%(v/v)正辛烷,色谱柱为Welch Materials XB-C_8(4.6 mm×200 mm,30μm),流速为1 m L·min~(-1),检测波长为220 nm,柱温为20℃。结果:白术内酯Ⅰ、Ⅲ在18 min内达到基线分离,白术内酯Ⅰ的线性范围为2.50~20.1μg·m L~(-1)(x~2=0.999 2),平均回收率(n=5)为97.89%(RSD=2.42%);白术内酯Ⅲ的线性范围为3.15~25.2μg·m L~(-1)(x~2=0.999 3),平均回收率(n=5)为98.61%(RSD=2.19%);检出限(LOD)分别为1.15、1.36 ng。对5个产地白术药材进行含量测定,得白术内酯Ⅰ的含量范围为0.106~0.217 mg·g~(-1),白术内酯Ⅲ的含量范围为0.169~0.389 mg·g~(-1)。通过优化最终微乳流动相的有机试剂(SDS、正丁醇、正辛烷)含量仅为12.7%。结论:经方法学验证,本法可用于白术药材中白术内酯Ⅰ、Ⅲ的质量分析。与传统HPLC法相比,MELC法采用微乳为流动相,既节约了有机试剂的用量,又减少了有机试剂的排放,具有绿色、经济的优点。
OBJECTIVE: To establish a new and stable microemulsion system and to simultaneously determine the content of atractylenolide I and III in Atractylodes macrocephala with microemulsion liquid chromatography. Methods: The main factors influencing the separation were investigated: surfactant, cosurfactant, oil phase, pH, temperature, column and so on. The microemulsion system was 3.3% (w / v) sodium dodecyl sulfate-8.25 The column was Welch Materials XB-C_8 (4.6 mm × 200 mm, 30 μm) with a flow rate of 1 m L · mL-1 (v / v) min -1, the detection wavelength was 220 nm and the column temperature was 20 ℃. RESULTS: Atractylolide Ⅰ and Ⅲ reached baseline separation within 18 min. The linear range of Atractylolide Ⅰ was 2.50 ~ 20.1 μg · m L -1 (x ~ 2 = 0.999 2). The average recovery (n (N = 5) was 97.89% (RSD = 2.42%). The linear range of atractylenolide Ⅲ was 3.15 ~ 25.2 μg · m L -1 (x ~ 2 = 0.999 3) Was 98.61% (RSD = 2.19%). The detection limits (LODs) were 1.15 and 1.36 ng respectively. The content of atractyloside I was determined to be from 0.106 to 0.217 mg · g -1 in Atractylodes macrocephala and the content of atractylodes lactone Ⅲ was 0.169-0.389 mg · g -1 . The organic reagent (SDS, n-butanol, n-octane) content was only 12.7% by optimizing the final microemulsion mobile phase. Conclusion: This method can be used for the quality analysis of Atractylodes a, Ⅲ in Atractylodes macrocephalae by methodological verification. Compared with the traditional HPLC method, the MELC method uses microemulsion as the mobile phase, which not only saves the amount of organic reagents but also reduces the emission of organic reagents, which has the advantages of being green and economical.