山药麸炒前后有效成分含量及UPLC指纹图谱差异性研究

Study on the content and UPLC fingerprint of Dioscoreae Rhizoma before and after processing

目的建立山药药材和麸炒山药饮片的UPLC指纹图谱及有效成分尿囊素、腺苷的含量测定方法,为山药及麸炒山药质量控制提供依据。方法采用HPLC法建立尿囊素质量分数测定方法,以Waters SPHERISORB NH2(250 mm×4.6 mm,5μm)为色谱柱,乙腈-水(体积比90∶10)为流动相,流速为1.0 mL/min,柱温为30℃,检测波长为224 nm;采用UPLC法建立腺苷的指纹图谱及质量分数测定方法,以YMC Triart(100 mm×2.1 mm,1.9μm)为色谱柱,乙腈-0.2%磷酸为流动相(梯度洗脱),流速为0.20 mL/min,柱温为30℃,检测波长为258 nm。结果10批山药生品标定5个共有峰,炮制品为8个共有峰;10批山药麸炒前后尿囊素及腺苷质量分数的差异不具有统计学意义。结论建立的方法为山药及麸炒山药饮片质量控制提供了一定的参考。

Objective To establish the methods for content determination and fingerprint of Dioscoreae Rhizoma and fried Dioscoreae Rhizoma and provide basis for quality control of Dioscoreae Rhizoma and fried Dioscoreae Rhizoma.Methods A method for the determination of allantoin was established by HPLC.The chromatographic column was Waters SPHERISORB NH2 column(250 mm×4.6 mm,5μm),acetylene-water(90∶10)was used as mobile phase with gradient elution.The flow rate was 1.0 mL/min,the column temperature was 30℃,and the detection wavelength was set at 224 nm.Determination of adenosine and specific chromatogram were accessed by using YMC Triart column(100 mm×2.1 mm,1.9μm),acetylene-0.2%phosphoric acid as mobile phase with gradient elution.The flow rate was 0.2 mL/min,the column temperature was 30℃,and the detection wavelength was set at 258 nm.Results There were 5 common peaks in 10 batches of Dioscoreae Rhizoma and 8 common peaks in processed products.The statistical results showed that there was no significant difference in the content of adenosine and allantoin of Dioscoreae Rhizoma before and after processing.Conclusion The established method provides a certain reference for the quality control of Dioscoreae Rhizoma and fried Dioscoreae Rhizoma.