郁金配方颗粒HPLC指纹图谱及指标成分含量测定研究

HPLC Fingerprint and Content Determination of Target Components of Yujin Dispensing Granules

目的采用高效液相色谱(HPLC)法同时测定郁金配方颗粒中2种指标成分的含量,并建立该制剂的HPLC指纹图谱。方法色谱柱为WelchUltimate AQ-C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸二氢钾溶液(梯度洗脱),流速为0.8 m L/min,检测波长为260 nm,柱温为30℃。采用"中药色谱指纹图谱相似度软件(2012.130723版)"进行相似度评价,并确定共有峰。结果15批煎剂及4批样品的HPLC图谱中有3个共有峰,1号峰为尿苷,3号峰为腺苷,相似度均大于0.85。尿苷、腺苷进样量分别在5.1~264.4 ng(r=0.9997)和15.9~792.6 ng(r=0.9997)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.00%(n=6),平均加样回收率分别为93.65%及93.51%,RSD分别为1.84%及2.03%(n=6)。结论该方法操作简便、准确,重复性好,结合所建立的指纹图谱,可为郁金配方颗粒的质量评价提供参考。

Objective To simultaneously determine the contents of the two target components of Yujin Dispensing Granules by the high-performance liquid chromatography(HPLC)method,and to establish an HPLC fingerprint of the preparation.Methods The chromatographic column was Welch Ultimate AQ-C18 column(250 mm×4.6 mm,5μm),the mobile phase was methanol(A)-0.1%potassium dihydrogen phosphate solution with gradient elution,the flow rate was 0.8 m L/min,the detection wavelength was 260 nm,and the column temperature was 30℃.The Similarity Evaluation System for Chromatographic Fingerprint of TCM(version 2012.130723)software was used to evaluate the similarity and to determine the common peaks.Results There were three common peaks in the HPLC chromatograms of 15 batches of Curcumae Radix decoction and 4 batches of samples with similarities higher than 0.85,the peakⅠwas uridine and peakⅢwas adenosine.The linear ranges of uridine and adenosine were 5.1-264.4 ng(r=0.9997)and 15.9-792.6 ng(r=0.9997),respectively.The RSDs of the precision,stability and repeatability tests were less than 2.00%(n=6),and the average recoveries of uridine and adenosine were 93.65%(RSD=1.84%,n=6)and 93.51%(RSD=2.03%,n=6),respectively.Conclusion The method is simple,accurate and reproducible,which can provide a reference for the quality evaluation of Yujin Dispensing Granules.