摘要
目的建立同时测定喜树果中喜树碱和10-羟喜树碱的高效液相色谱方法,并建立其HPLC指纹图谱。方法样品经75%甲醇-盐酸溶液超声提取,采用Agilent ZORBAX Eclipse XDB-C_(18)(250 mm×4.6 mm,5μm)色谱柱,0.01%磷酸溶液-甲醇梯度洗脱,流速:0.8 mL·min^(-1),柱温:30℃,检测波长:266 nm。对9批不同产地喜树果药材进行分析。结果方法线性关系良好(R^(2)=1.0000)。喜树碱平均回收率96.5%,RSD=0.7%(n=9);10-羟喜树碱平均回收率99.4%,RSD=1.1%(n=9)。9批喜树果中喜树碱含量在0.583~1.016 mg·g^(-1),10-羟喜树碱含量在0.099~0.195 mg·g^(-1)。指纹图谱有8个特征峰,9批药材相似度均大于0.9。结论该方法精密度好、准确度高,可为喜树果的质量标准完善提供参考。
OBJECTIVE To establish a high-performance liquid chromatography(HPLC)method for determination of camptothecin and 10-hydroxycamptothecin in Camptothecae acuminatae fructus.And establish its HPLC fingerprint spectrum.METHODS The test samples were extracted by ultrasound with 75%methanol-hydrochloric acid solution(volume ratio 100∶1),separated on Agilent ZORBAX Eclipse XDB-C_(18)column(250 mm×4.6 mm,5μm),and eluted with a gradient of 0.01%phosphoric acid solution and methanol.Flow rate:0.8 mL·min^(-1).Column temperature:30℃.Wavelength:266 nm.Validate the HPLC method and analyze 9 samples from different origins.RESULTS The method showed a good linear relationship(R^(2)=1.0000).The average recoveries of camptothecin was 96.5%,RSD=0.7%(n=9),and 10-hydroxy camptothecin was 99.4%,RSD=1.1%(n=9).The content of camptothecin in 9 batches of camptothecin fruits ranges from 0.583-1.016 mg·g^(-1),and the content of 10-hydroxy camptothecin ranges from 0.099-0.195 mg·g^(-1).The fingerprint spectrum has 8 characteristic peaks,and the similarity of 9 samples were all greater than 0.9.CONCLUSION The method has the advantages good precision,and high accuracy.It provides experimental basis for the quality evaluation and quality standard improvement of Camptothecae acuminatae fructus.
作者
张欣
陈雅念
周心怡
吴晓敏
ZHANG Xin;CHEN Ya-nian;ZHOU Xin-yi;WU Xiao-min(Three Gorges Public Inspection and Testing Center,Yichang 443000,China)
出处
《海峡药学》
2025年第4期20-24,共5页
Strait Pharmaceutical Journal
基金
宜昌市自然科学研究项目(No.A23-2-034)。
关键词
喜树果
喜树碱
10-羟喜树碱
高效液相色谱
指纹图谱
Camptothecae acuminatae fructus
Camptothecin
10-hydroxy camptothecin
HPLC
Fingerprint
