LC-MS、MS法对血栓通注射液中皂苷成分快速定量分析.docx
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【摘要】目的:建立LC-MS/MS方法快速测定血栓通注射液中5种皂苷成分。方法:色谱柱为BEHC18(2.1mm*100mm,1.8μm),流速为0.400mL/min,流动相为乙腈-水,洗脱方式为梯度洗脱,柱温为30℃,进样量为2μL;采用多重反应监测模式(MRM)下负离子扫描方式,离子源为ESI-。结果:人参皂苷Rg1、人参皂苷Rb1、人参皂苷Re、人参皂苷Rd及三七皂苷R1在浓度范围内线性关系良好,R20.999,定量限在0.34~1.45ng/mL;低、中、高3种浓度水平加样回收率在90.59%~104.10%,相对标准偏差为1.27%~4.29%;进样精密度为1.80%~2.64%。结论:本研究成功建立血栓通注射液中5种皂苷成分LC-MS/MS定量分析方法,方法操作简单,准确度和精密度良好,并完成不同厂家不同批次血栓通注射液中5种皂苷成分测定。
【关键词】LC-MS/MS;血栓通注射液;人参皂苷Rg1;人参皂苷Rb1;人参皂苷Re;人参皂苷Rd;三七皂苷R1
LC-MS/MSmethodforrapidquantitativeanalysisofsaponincomponentsinXueshuantonginjection
ZHANGXiaojun1,FUHuihui2
1.GuangdongLeiyunshangPharmaceuticalCo.,Ltd,Yunfu,Guangdong527300,China;2.YunfuTraditionalChineseMedicineHospital,Yunfu,Guangdong527300,China
【Abstract】Objective:ToestablishaLC-MS/MSmethodforrapiddeterminationoffivesaponincomponentsinXueshuantonginjection.Methods:ThechromatographiccolumnwasBEHC18(2.1mm*100mm,1.8μm),withaflowrateof0.400mL/min,themobilephasewasacetonitrilewater,theelutionmethodwasgradientelution,thecolumntemperaturewas30℃,andtheinjectionvolumewas2μL;Adoptingthenegativeionscanningmethodundermultiplereactionmonitoringmode(MRM),andtheionsourcewasESI-.Results:ThelinearrelationshipbetweenginsenosideRg1,ginsenosideRb1,ginsenosideRe,ginsenosideRd,andnotoginsenosideR1wasgoodwithintheconcentrationrange,withR20.999,andthequantificationlimitsofthefivesaponincomponentswerefrom0.34to1.45ng/mL;Therecoveryratesofthefivesaponincomponentsatlow,medium,andhighconcentrationlevelsrangedfrom90.59%to104.10%,andtherelativestandarddeviationwasfrom1.27%to4.29%;Theprecisionofinjectionwerebetween1.80%and2.64%.Conclusion:ThisstudysuccessfullyestablishedaLC-MS/MSquantitativeanalysismethodforfivesaponincomponentsinXueshuantonginjection.Themethodissimpletooperate,withgoodaccuracyandpreci