HPLC-ELSD法同时测定生白术中的D-果糖、D-葡萄糖和蔗糖

Simultaneous determination of D-fructose,D-glucose and sucrose in Atractylodes macrocephala Koidz. by HPLC-ELSD

目的建立HPLC-ELSD法同时测定生白术中D-果糖、D-葡萄糖和蔗糖的含有量,并对不同产地（浙江、安徽和湖北省）及批次药材中的这3种成分进行分析。方法生白术提取物的分析采用Waters XBridgeTMAmide色谱柱（4.6 mm×250 mm,3.5μm）;流动相为乙腈-水（80∶20）;体积流量1.0 m L/min;柱温40℃。质谱测定采用电喷雾离子源（ESI）的飞行时间质谱（TOF/MS）;负离子模式;质量扫描范围m/z 50~800。结果 D-果糖在7.943~18.53μg、D-葡萄糖在0.583 5~1.362μg、蔗糖在1.415~3.302μg范围内均呈良好的线性关系（r〉0.998）,其平均回收率分别为101.4%、100.1%、102.0%,RSD分别为1.3%、1.8%、1.3%（n=9）。在10批生白术药材中,D-果糖含有量为9.946~45.83 mg/g、D-葡萄糖为1.198~7.743 mg/g、蔗糖为5.231~15.76 mg/g。结论不同产地及批次生白术中的含有量依次为D-果糖〉蔗糖〉D-葡萄糖,并且差异较明显。

AIM To establish a method for simultaneously determining D-fructose,D-glucose and sucrose in Atractylodes macrocephala Koidz. by HPLC-ELSD and analyze these three constituents in different growing areas（ Zhejiang,Anhui and Hubei Province） and batches of this plant. METHODS The analysis of Atractylodes macrocephala Koidz. extract was performed on Waters XBridge^TMamide column（ 4. 6 mm × 250 mm,3. 5 μm）,mobile phase was acetonitrile-water（ 80 ∶ 20）,flow rate was 1. 0 m L / min,and column temperature was maintained at 40℃. Time-of-flight mass spectrometer（ TOF / MS） and electro-spray ion source（ ESI） were used for qualitative analysis in a negative ion mode,and mass scan range was m / z 50- 800. RESULTS Good linear relationships were in the ranges of 7. 943- 18. 53 μg for D-fructose,0. 583 5- 1. 362 μg for D-glucose and 1. 415- 3. 302 μg for sucrose（ r〉0. 998）. Their average recoveries were 101. 4%,100. 1% and 102. 0% with the RSDs of 1. 3%,1. 8% and 1. 3%,respectively（ n = 9）. In ten batches of Atractylode macrocephala Koidz.,the contents of Dfructose,D-glucose and sucrose were 9. 946- 45. 83 mg / g,1. 198- 7. 743 mg / g and 5. 231- 15. 76 mg / g,respectively. CONCLUSION The contents are in the order of D-fructose 〉sucrose 〉D-glucose in different growing areas and batches of Atractylodes macrocephala Koidz.,having obvious difference.