| 基于HPLC-TOF/MS与HPLC-MS/MS的养心氏片主要成分研究 |
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| 基金项目:国家自然科学基金项目（21575042） |
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| 中文摘要:采用高效液相色谱-高分辨飞行时间质谱联用技术(HPLC-TOF/MS)，建立了快速鉴定养心氏片化学成分的定性方法,并利用高效液相色谱-串联三重四极杆质谱(HPLC-MS/MS)对养心氏片的主要成分进行定量分析。HPLC-TOF/MS法以ZORBAX Eclipse Plus C18(100 mm×30 mm,18 μm)为色谱柱，乙腈-01%甲酸为流动相，梯度洗脱，流速为02 mL·min-1，柱温30 ℃，质谱采用正、负离子扫描，可推断鉴定养心氏片中的30种成分。HPLC-MS/MS 法采用Waters XBridgeBEH C18(150 mm×46 mm,25 μm)为色谱柱，乙腈-01%甲酸为流动相，梯度洗脱，流速04 mL·min-1，柱温30 ℃，Scheduled MRM正负离子切换监测模式定量分析。对养心氏片中16种主要成分进行HPLC-MS/MS分析，16种成分的质量浓度与峰面积呈良好线性，相关系数r≥0997，检出限为0039 1~781 μg/L，定量下限为0156~312 μg/L，平均加标回收率为968%~1038%，相对标准偏差(RSD)为10%~35%。结果表明，该方法操作简便、结果准确、重复性好，可用于养心氏片中多组分的同时定性和定量分析，为养心氏产品的质量控制、药理研究和应用奠定了基础。 |
| 中文关键词:养心氏片；化学成分；HPLC-TOF/MS HPLC-MS/MS；定量分析 |
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| Investigation on Major Constituents in Yangxinshi Tablets Based on HPLC-TOF/MS and HPLC-MS/MS |
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| Abstract:A rapid method for the identification of constituents in Yangxinshi tablets was established by high performance liquid chromatography-time of flight mass spectrometry(HPLC-TOF/MS).Simultaneously,the quantitation on the sample was performed by high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS).30 kinds of constituents in Yangxinshi tablets were identified by HPLC-TOF/MS in the running conditions as follows:chromatographic column:an Agilent ZORBAX Eclipse Plus C18 column(100 mm×30 mm,18 μm),mobile phase:acetonitrile-01% formic acid solution,elution type:gradient elution,flow rate:02 mL·min-1,column temperature:30 ℃,MS scanning mode:electrospray in both positive and negative ion.The HPLC-MS/MS method was operated under the following conditions:chromatographic column:a Waters XBridge BEH C18 column(150 mm×46 mm,25 μm),mobile phase:acetonitrile-01% formic acid solution,elution type:gradient elution,flow rate:04 mL·min-1,column temperature:30 ℃,MS scanning mode:multiple reaction monitoring(MRM) mode with electrospray ion source in both positive and negative ion.16 main constituents in Yangxinshi tablets were determined by HPLC-MS/MS.There were excellent linear responses for the peak areas of the analytes to their concentrations with the correlation coefficients(r) not less than 0997.The limits of detection(LODs) and quantitation(LOQs) for 16 constituents were in the range of 0039 1-781 μg/L and 0156-312 μg/L,respectively.The average recoveries were in the range of 968%-1038% with the relative standard deviations of 10%-35%.With the advantages of simple operation,accuracy and acceptable reproducibility,the developed method could be applied in the qualitation and quantitation of constituents in Yangxinshi tablets.Therefore,it could provide a reference for the quality control,further study and application of Yangxinshi tablets. |
| Key Words:Yangxinshi tablets constituents HPLC-TOF/MS HPLC-MS/MS quantitative analysis |
| 引用本文：王静，蒋惠宇,张晶晶,张华,彭孝军.基于HPLC-TOF/MS与HPLC-MS/MS的养心氏片主要成分研究[J].分析测试学报,2018,37(7):759-765. |
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