| 超快速液相色谱－三重四极杆－线性离子阱质谱法同时测定桑寄生中多元活性成分 |
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| 基金项目:广西壮瑶药重点实验室开放课题（GXZYKF2020-2）；江苏省研究生科研创新计划（KYCX22_2019） |
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| 中文摘要:建立了超快速液相色谱－三重四极杆－线性离子阱质谱（UFLC－QTRAP－MS/MS）同时测定桑寄生中黄酮类、有机酸类、核苷类和氨基酸类共33种活性成分含量的方法，并对不同寄主的桑寄生茎枝和叶进行比较分析。通过Box－Behnken响应面法优化供试品制备条件；采用XBridge?C18（4.6 mm × 100 mm，3.5 μm）色谱柱进行分离，以0.1%甲酸水－甲醇为流动相进行梯度洗脱；质谱采用电喷雾离子源（ESI），以多反应监测（MRM）模式进行检测。结果表明，最佳制备条件为甲醇体积分数70%，液料比（mL∶g）31∶1，提取时间32 min。33种目标成分在相应质量浓度范围内的线性关系良好，相关系数（r）均不低于0.999 0；检出限（LOD）和定量下限（LOQ）分别为0.13 ~ 66.85 ng/mL和0.42 ~ 222.83 ng/mL；平均加标回收率为98.0% ~ 101%，相对标准偏差（RSD）均小于4.0%。所构建的方法准确、稳定，可为桑寄生药材质量的综合评价和全面控制提供新的方法参考，也为桑寄生的合理开发利用提供了依据。 |
| 中文关键词:桑寄生 超快速液相色谱－三重四极杆－线性离子阱质谱 独立样本t检验 相关性分析 Box－Behnken响应面法 活性成分 |
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| Simultaneous Determination of Multiple Active Constituents in Taxilli Herba by UFLC－QTRAP－MS/MS |
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| Abstract:An ultra-fast liquid chromatography－triple quadrupole－linear ion trap mass spectrometry （UFLC－QTRAP－MS/MS） method was developed for the simultaneous determination of 33 active constituents consisting of flavonoids，organic acids，nucleosides，and amino acids in Taxilli Herba．The stems branches and leaves of Taxilli Herba from different hosts were also compared and analyzed．The optimum conditions for the preparation of the test solution were selected by the Box－Behnken response surface method（BBD－RSM）．The target constituents were separated on an XBridge? C18（4.6 mm × 100 mm，3.5 μm） analytical column by gradient elution using 0.1% formic acid aqueous solution and methanol as mobile phases，then analyzed by mass spectrometry with an electrospray ion source（ESI） in multi reaction monitoring（MRM） mode，and finally quantified by the external standard method．The correlation analysis and independent sample t-test were performed for the contents of the 33 target constituents．The results showed that the optimal extraction conditions were as follows：a methanol volume fraction of 70%，a liquid to material ratio （mL∶g） of 31∶1 and an extraction time of 32 min，under which the extraction yield for quercetrin reached 3.77 mg/g．The standard curves for 33 target constituents showed good linearity in the corresponding range with their correlation coefficients（r） not less than 0.999 0．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.13－66.85 ng/mL and 0.42－222.83 ng/mL，respectively．The precision，repeatability and stability of this method were excellent．The average recoveries at low，medium and high spiked levels in real samples ranged from 98.0% to 101%，with the relative standard deviations（RSDs） all less than 4.0%．The correlation analysis revealed that the contents of active constituents were associated to a certain extent．A t-test revealed that the contents of various active constituents in the stems branches and leaves of Taxilli Herba differed significantly，and the contents of each constituent，such as quercetin-3-O-glucuronide，hyperin，rutin，isoquercitrin，quercetrin and auicularin，were significantly higher in the leaves than in the stems and branches．The developed method is accurate and stable，which could provide a new method reference for the comprehensive evaluation and overall control on the quality of Taxilli Herba，and a certain reference basis for its rational exploitation． |
| Key Words:Taxilli Herba ultra-fast liquid chromatography－triple quadrupole－linear ion trap mass spectrometry independent samples t-test correlations Box－Behnken response surface methodology active constituents |
| 引用本文：吴楠，袁嘉欢，王文辛，刘训红，黎理，殷圣鑫，陈海杰，薛佳，周永逸，杨薇.超快速液相色谱－三重四极杆－线性离子阱质谱法同时测定桑寄生中多元活性成分[J].分析测试学报,2022,41(8):1153-1162. |
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