南大青叶薄层色谱法鉴别的完善与HPLC法含量测定的建立  

Improvement of TLC identification and establishment of HPLC assay for Leaves of Baphicacanthus cusia(Nees)Bremek

作　　者：刘主洁 张伟[1] 卢秋梅 侯惠婵[1] 顾利红[1] 张丹雁[2] 曾云保 欧阳志 LIU Zhujie;ZHANG Wei;LU Qiumei;HOU Huichan;GU Lihong;ZHANG Danyan;ZENG Yunbao;OUYANG Zhi(Guangzhou Institute for Drug Control,NMPA Key Laboratory for Quality Evaluation of Traditional,Chinese Medicine,Guangzhou 510160,China;Guangzhou University of Chineses Medicine,Guangzhou 510006,China;Guangzhou Lifetech Pharmaceutical Co.,Ltd.,Guangzhou 510990,China;South China University of Technology Hospital,Guangzhou 510641,China)

机构地区：[1]广州市药品检验所/国家药监局中成药质量评价重点实验室,广州510160 [2]广州中医药大学,广州510006 [3]广州莱泰制有限公司,广州510990 [4]华南理工大学医院,广州510641

出　　处：《中国药品标准》2021年第1期37-42,共6页Drug Standards of China

摘　　要：目的:提高南大青叶的质量标准,对其质量进行更有效控制。方法:以靛蓝、靛玉红为对照品,通过薄层色谱法(TLC)对南大青叶进行定性分析;采用高效液相色谱法(HPLC)对靛蓝进行含量测定,以十八烷基硅烷键合硅胶为填充剂;以乙腈(A)-水(B)为流动相,梯度洗脱(0~10 min,5%→60%A;10~20 min,60%A);流速为1.0 mL·min^(-1);检测波长为289 nm。结果:TLC斑点清晰,分离度高,方法耐用性好,能区分南大青叶及其混伪品广西马蓝;HPLC法含量测定结果显示,靛蓝在24.98~249.8 ng线性关系良好(r=0.9995,n=6),加样回收率为100.80%,RSD=1.8%,n=6。测定样品11批,结果靛蓝的含量范围为0.52%~0.92%。结论:所建立的薄层色谱鉴别方法专属性好,能有效鉴别该药材中靛蓝及靛玉红成分;HPLC方法分离度好、稳定可靠,可有效控制南大青叶药材的质量,为该药材的合理开发利用提供参考。Objective:To improve the specification and optimize the test methods for Leaves of Baphicacanthus cusia(Nees)Bremek.Methods:Thin layer chromatography(TLC)was performed for identification of leaves of Baphicacanthus cusia(Nees)Bremek with Indigotin and Indirubin RS as the control.Indigotin was determined by high performance liquid chromatography(HPLC).The test was performed in octadecylsilane chemically bonded silica column under the gradient elution of acetonitrile(phase A)and water(phase B).The gradient programme was follow:0-10 min,5%→60%phase A;10-20 min,60%phase A.The flow rate was 1.0 mL·min^(-1),and the detection wavelength was 289 nm.Results:The TLC spots were clear and the resolutions were good.The improved method had the good robustness and could distinguish Leaves of Baphicacanthus cusia(Nees)Bremek and Pteracanthus guangxiensis.There was a good linear relationship for indigotin in the range of 24.98-249.8 ng(r=0.9995,n=6),and the spiked average recovery was 100.80%with the RSD of 1.8%(n=6).The contents of indigotin in 11 batches of samples were 0.52%-0.92%.Conclusion:The improved TLC method has the good specificity and can identify the components of Indigotin and indirubin effectively.HPLC method has good resolution and reliability.It can be applied for quality control of Leaves of Baphicacanthus cusia(Nees)Bremek.effectively.

关 键 词：南大青叶 薄层色谱法 高效液相色谱法 靛蓝 靛玉红 

分 类 号：R921.2[医药卫生—药学]