不同贮存时间对酸橙枳实药材的质量影响

Effects of Different Storage Time on the Quality of Immature Fruit of Citrus Aurantium

目的:建立同时测定枳实中芸香柚皮苷、柚皮苷、野漆树苷、橙皮苷、新橙皮苷和川陈皮素含量的方法,并初步探讨贮存时间对酸橙枳实药材质量的影响。方法:(1)建立超高效液相色谱法同时检测不同贮存时间酸橙枳实药材中黄酮类化合物芸香柚皮苷、柚皮苷、野漆树苷、橙皮苷、新橙皮苷和川陈皮素的含量。色谱条件为,WATERS ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm);水(含0.2%冰醋酸)-乙腈梯度洗脱流动相;检测波长330 nm;柱温30℃;流速0.3 ml/min。(2)高效液相色谱法检测相同样品中辛弗林的含量。色谱条件为,Agilent TC-C18色谱柱(4.6 mm×250 mm,5μm),甲醇-水(水中含磷酸二氢钾0.06%,十二烷基磺酸钠0.1%,冰醋酸0.1%)(V∶V=1∶1)为流动相;流速1.0 ml/min;柱温30℃;检测波长275 nm。结果:超高效液相色谱法检测黄酮类化合物,高效液相色谱法检测辛弗林含量,方法精密度、重复性、稳定性和加样回收率良好,可用于样品的含量测定。枳实中芸香柚皮苷、野漆树苷、橙皮苷、川陈皮素及辛弗林含量与贮存时间无明显规律性。随贮存时间延长,柚皮苷含量有升高趋势,新橙皮苷含量有降低趋势。结论:建立了超高效液相色谱法同时测定枳实中芸香柚皮苷、柚皮苷、野漆树苷、橙皮苷、新橙皮苷和川陈皮素含量的方法。针对不同产地的7年内不同贮存时间的样品,以黄酮类成分和辛弗林含量为评价指标的酸橙枳实药材的质量未见明显差异。

OBJECTIVE:To establish the simultaneous determination method for flavonoids contents of narirutin,naringin,rhoifolin,hesperidin,neohesperidin and nobiletin in immature fruit of citrus aurantium,and to probe into the effects of different storage time on the quality of immature fruit of citrus aurantium.METHODS:(1)Ultra-high performance liquid chromatography(UPLC)was used to detect the flavonoids contents of narirutin,naringin,rhoifolin,hesperidin,neohesperidin and nobiletin in immature fruit of citrus aurantium.The WATERS ACQUITY UPLC HSS T3 chromatographic column(2.1 mm×100 mm,1.8μm)was used.Water(containing 0.2%acetic acid)-acetonitrile was used as mobile phase,with gradient elution.The detection wavelength was 330 nm,the column temperature was 30℃,with flow rate of 0.3 ml/min.(2)High-performance liquid chromatography(HPLC)was used to detect the content of synephrine in immature fruit of citrus aurantium.The Agilent TC-C18 chromatographic column(4.6 mm×250 mm,5μm)was used,methanol-water(0.06%potassium dihydrogen phosphate in water,0.1%sodium dodecylsulfonate,0.1%glacial acetic acid)(V∶V=1∶1)was used as the mobile phase,the flow rate was 1.0 ml/min,the column temperature was 30℃and the detection wavelength was 275 nm.RESULTS:UPLC can be used to detect flavonoids compounds,and HPLC can be used to detect synephrine.The method has better precision,repeatability,stability and sample recovery,and can be used for the determination of the content of the sample.There is no obvious regularity in the contents of narirutin,rhoifolin,hesperidin,nobiletin and synephrine in immature fruit of citrus aurantium.With the prolonged storage time,the naringin content increased and the neohesperidin content decreased.CONCLUSIONS:The UPLC method of simultaneous determination about the flavonoids contents of narirutin,naringin,rhoifolin,hesperidin,neohesperidin and nobiletin in immature fruit of citrus aurantium was developed.According to the samples of different origin and storage time within 7 years,there was no significant difference in the quality of citrus aurantium with flavonoids and synephrine content as evaluation indicators.