HPLC Fingerprinting and Spectrum-antitumor Effect Relationship for Discrimination between Mylabris phalerata Pallas and Mylabris cichorii Linnaeus

Objective： Evaluation of discrimination between two Mylabris Species based on HPLC fingerprinting andspectrum-antitumor effect relationship. Methods： In this study, a simple and efficient high-performance liquidchromatography （HPLC） method integrating with chemometric analysis and spectrum-antitumor effect relationship wasdeveloped for discrimination between two species of Mylabris： Mylabris phalerata Pallas （MP） and Mylabris cichoriiLinnaeus （MC）. Results： In the fingerprint analysis, 14 characteristic peaks were selected to assess the differencesbetween MP and MC using the similarity and pattern recognition analysis using PCA and OPLS-DA. The HPLCchromatograms of samples from 10 regions of China showed differences between MP and MC, and 7 characteristicchemical markers were found. In the spectrum-antitumor effect relationship analysis, 4 activity markers played a vitalrole in decreasing the IC50 and might be the antitumor components of Mylabris by grey relational analysis andmultivariate linear regression analysis. The chemometric analysis in combination with spectrum-effect relationshipresults indicated that peaks 2 （cytosine）, 4 （unknown） and 14 （unknown） were important differential markers fordistinguishing the two species of Mylabris. Conclusion： The method is applicable, credible and more efficient todiscriminate MP and MC, and will offer a new way for facilitating quality control of insect medicines.

不同产地与品种斑蝥中化学成分的GC-MS分析

运用气相色谱-质谱联用技术分析了7种不同产地和品种的斑蝥(Mylabris)所含化学组分,共鉴定出12种组分,其中4种成分均在所有斑蝥中检出。结果表明,不同产地与品种斑蝥的化学成分组成既有共性,又有自身的独特性。

大斑芫菁挥发性成分的气相色谱-质谱联用分析

采用水蒸气蒸馏法提取大斑芫菁(Mylabris phalerata Pallas)的挥发性成分,并采用气相色谱-质谱联用技术对其进行了分析鉴定,旨在为大斑芫菁的综合利用提供理论依据。从大斑芫菁中共检出86种挥发性成分,并鉴定出其中的41种,以醇、醛、酮、酸类物质居多。其中相对百分含量较高的有苯乙醛(4.07%)、油酸(3.21%)、1,13-十四碳二烯(2.22%)、芳樟醇(1.70%)、香叶基丙酮(1.64%)。

黑黄小斑蝥中挥发性化学成分的SPME-GC-MS分析

采用固相微萃取-气相色谱-质谱联用技术(SPME-GC-MS)分析黑黄小斑蝥(Mylabris cichorii Linnaeus)挥发性成分的方法。SPME的萃取头为100μm PDMS,样品用量为0.4 g,平衡及吸附温度为80℃,平衡时间为30 min,吸附时间为15 min,解吸时间为2 min。从斑蝥样品中分离得到21个色谱峰,鉴定出11个化合物,其中共有峰为斑蝥素、环己甲醇、十三烷、环己醇和1,13-十四碳二烯,但产地间成分和含量差异较大。该法可用于斑蝥挥发性成分的快速分析,为评价斑蝥质量提供参考。

UPLC法测定黄黑小斑蝥中的斑蝥素

建立一种超高效液相色谱法(UPLC)测定斑蝥素的含量,同时比较了野生与人工饲养黄黑小斑蝥(Mylabris cichorii Linnaeus)中斑蝥素含量差异。前处理以1%盐酸/丙酮作溶剂,超声提取斑蝥素;采用C_(18)为分析柱,流动相为乙腈-水(40∶60),紫外检测波长为230 nm,流速0.2 mL/min,柱温35℃,进样量2μL。结果表明,斑蝥素在0.02~1.00 mg/mL线性关系良好(R^(2)=0.9999);不同加标水平下平均回收率为97.9%~100.9%,RSD在1.7%~3.8%。采用该法测得野生斑蝥斑蝥素含量为3.080%,人工饲养斑蝥斑蝥素含量为1.680%,两者均高于药典中斑蝥药材的斑蝥素含量不得少于0.35%的要求。该方法准确、可靠,适用于斑蝥中斑蝥素的测定,人工饲养黄黑小斑蝥亦可用作斑蝥素的来源药材。