银杏叶片中5种银杏双黄酮类成分同时测定方法的建立  

Establishment of determination method for five Ginkgo biflavones in Ginkgo biloba leaves tablets

作　　者：刘丽娜[1] 李海亮 李耀磊[1,2] 金红宇 昝珂[1] LIU Lina;LI Hailiang;LI Yaolei;JIN Hongyu;ZAN Ke(National Institutes for Food and Drug Control,Beijing 100050,China;College of TCM,Beijing University of Chinese Medicine,Beijing 100029,China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]北京中医药大学中药学院,北京100029

出　　处：《中国药房》2022年第10期1220-1224,共5页China Pharmacy

摘　　要：目的建立同时测定银杏叶片中穗花杉双黄酮、白果黄素、银杏双黄酮、异银杏双黄酮、金松双黄酮含量的方法。方法银杏叶片经甲醇超声提取后,采用超高效液相色谱法测定。以Waters Acquity UPLC HSS T3为色谱柱,以乙腈-0.4%磷酸溶液为流动相进行梯度洗脱,流速为0.4 mL/min,柱温为35℃,检测波长为340 nm,进样量为1μL(对照品)、10μL(供试品)。采用一测多评法,以穗花杉双黄酮为参照物,计算白果黄素、银杏双黄酮、异银杏双黄酮、金松双黄酮的相对校正因子,以相对保留时间法定位色谱峰,再计算上述成分的含量并与外标法测定结果(穗花双黄酮除外)进行比较。结果穗花杉双黄酮、白果黄素、银杏双黄酮、异银杏双黄酮、金松双黄酮检测进样量的线性范围分别为0.10~8.21、0.24~19.34、0.16~12.98、0.22~17.66、0.06~4.86 ng(r均大于0.999),定量限分别为0.10、0.24、0.16、0.22、0.06 ng;精密度、重复性、稳定性(36 h)试验的RSD均小于3.00%,平均加样回收率为99.77%~102.85%,RSD为1.90%~4.40%(n=6)。白果黄素、银杏双黄酮、异银杏双黄酮、金松双黄酮的平均相对校正因子分别为0.91、0.93、0.96、0.95,平均相对保留时间分别为1.08、1.18、1.19、1.30;一测多评法计算结果与外标法测得结果的相对偏差在±3.00%以内。结论所建方法准确、稳定,可用于银杏叶片中银杏双黄酮类成分的测定及质量控制。OBJECTIVE To establish a method for the determination of amentoflavone,bilobetin,ginkgetin,isoginkgetin and sciadopitysin in Ginkgo biloba leaves tablets.METHODS After extracted with methanol,ultra-performance liquid chromatography(UPLC)was adopted to determine G.biloba leaves tablets.The determination was performed on Waters Acquity UPLC HSS T3column with acetonitrile-0.4%phosphoric acid as mobile phase(gradient elution)at the flow rate of 0.4 mL/min.The column temperature was set at 35℃,and the detection wavelength was 340 nm.The sample size were 1μL(substance control)and 10μL(test sample).The relative correction factors(RCFs)of bilobetin,ginkgetin,isoginkgetin and sciadopitysin were calculated by quantitative analysis of multicomponents by single marker(QAMS)using amentoflavone as control.The chromatographic peak was located with the relative retention time method.Then the contents of the above components were calculated,and the results were compared with those of external standard method(ESM)(except for amentoflavone).RESULTS The linear ranges of amentoflavone,bilobetin,ginkgetin,isoginkgetin and sciadopitysin were 0.10-8.21,0.24-19.34,0.16-12.98,0.22-17.66,0.06-4.86ng,respectively(all r>0.999).The quantitation limits were 0.10,0.24,0.16,0.22,0.06 ng,respectively.RSDs of precision,repeatability and stability tests(36 h)were all lower than 3.00%.The average recoveries were 99.77%-102.85%,and RSDs were1.90%-4.40%(n=6).The average RCFs of bilobetin,ginkgetin,isoginkgetin and sciadopitysin were 0.91,0.93,0.96 and 0.95,respectively.The average relative retention times were 1.08,1.18,1.19 and 1.30,respectively.The relative deviation between the calculation result of QAMS and ESM was within±3.00%.CONCLUSIONS The established method is accurate and stable,and can be applied to the determination of Ginkgo biflavones in G.biloba leaves tablets and control the quality.

关 键 词：超高效液相色谱法 一测多评法 银杏叶片 银杏双黄酮 含量测定 

分 类 号：R917[医药卫生—药物分析学]