舒血宁注射液中15种黄酮醇苷测定及其UPLC指纹图谱建立

Determination of fifteen flavonol glycosides in Shuxuening Injection and establishment of its UPLC fingerprints

目的测定舒血宁注射液中槲皮素3-O-(2″,6″-α-L-二鼠李糖)-β-D-葡萄糖、杨梅素3-O-芸香糖苷、槲皮素3-O-α-L-鼠李糖-2″-(6-对香豆酰基)-β-D-葡萄糖-7-O-β-D-葡萄糖苷、山柰酚3-O-(2″,6″-α-L-二鼠李糖)-β-D-葡萄糖、异鼠李素3-O-(2″,6″-α-L-二鼠李糖)-β-D-葡萄糖、芦丁、3′-甲基杨梅素-3-O-芸香糖苷、异槲皮苷、槲皮素3-O-(2″-β-D-葡萄糖)-α-L-鼠李糖苷、山柰酚3-O-芸香糖苷、水仙苷、丁香亭3-O-芸香糖苷、山柰酚3-O-(2″-β-D-葡萄糖)-α-L-鼠李糖苷、槲皮素3-O-[2′-O-(6″-O-对羟基-反式-香豆酰基)-D-葡萄糖基]-α-L-鼠李糖苷、山柰酚3-O-[2′-O-(6″-O-对羟基-反式-香豆酰基)-D-葡萄糖基]-α-L-鼠李糖苷的含量,并建立其UPLC指纹图谱。方法该药物70%甲醇溶液的分析采用Agilent Zorbax SB-C_(18)色谱柱(3.0 mm×150 mm,1.8μm);流动相乙腈-0.1%甲酸,梯度洗脱;体积流量0.35 mL/min;柱温40℃;检测波长360 nm。结果15种黄酮醇苷在各自范围内线性关系良好(R^(2)>0.9990),平均加样回收率97.00%~102.80%,RSD 0.46%~3.22%。10批样品指纹图谱中有23个共有峰,相似度均大于0.990。结论该方法简便准确,重复性好,可为舒血宁注射液的全面质量评价提供依据。

AIM To determine the contents of querceti-3-O-(2″,6″-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside,myricetin-3-O-rutinoside,quercetin-3-O-α-L-[6-p-coumaroyl-(β-D)-glucopyranosyl-(1,2)-rhamnopyranoside]-7-O-β-D-glucopyranoside,kaempferol-3-O-(2″,6″-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside,isorhamnetinl-3-O-(2″,6″-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside,rutin,myricetin-3′-methyl ether-3-O-rutinoside,isoquercitrin,querceti-3-O-β-D-glucopyranosyl-(1→2)-α-L-rhamnopyranoside,kaempferol 3-O-rutinoside,narcissoside,myricetin-3′,5′-dimethyl ether-3-O-rutinoside,kaempferol-3-O-β-D-glucopyranosyl-(1→2)-α-L-rhamnopyranoside,quercetin-3-O-[2-O-(6-O-p-hydroxyl-E-coumaroyl)-D-glucosyl]-(1-2)-L-rhamnoside and kaempferol-3-O-[2-O-(6-O-p-hydroxyl-E-coumaroyl)-D-glucosyl]-(1-2)-L-rhamnoside in Shuxuening Injection,and to establish the UPLC fingerprints.METHODS The analysis of 70% methanol solution of this drug was performed on a 40℃ thermostatic Agilent Zorbax SB-C_(18) column(3.0 mm×150 mm,1.8μm),with the mobile phase comprising of acetonitrile-0.1% formic acid flowing at 0.35 mL/min in a gradient elution manner,and the detection wavelength was set at 360 nm.RESULTS Fifteen flavonol glycosides showed good linear relationships within their own ranges(R^(2)>0.9990),whose average recoveries were 97.00%-102.80% with the RSDs of 0.46%-3.22%.There were twenty-three common peaks in the fingerprints for ten batches of samples with the similarities of more than 0.990.CONCLUSION This simple,accurate and reproducible method can provide a basis for the comprehensive quality evaluation of Shuxuening Injection.