摘要
目的:研究建立运用高效液相色谱-串联质谱法(LC-MS/MS)同时测定血塞通注射液中人参皂苷Rg1、人参皂苷Rb1、 人参皂苷Re、 人参皂苷R、 三七皂苷R1的定性定量方法,用于血塞通注射液的质量控制.方法:采用CAPCELL CORE C18色谱柱(2.1 mm×150 mm,2.7μm),柱温30℃,流动相:A(超纯水)和B(乙腈),使用梯度洗脱如下:0.01~3.00 min,95%A;3.00~4.00 min,95%A^30%A;4.00 min^10.00 min,30%A;10.00 min^12.00 min,30%A^95%A;12.00 min^15.00 min,95%A.流速设定为0.300 mL/min.总运行时间为15.0 min.采用多重反应监测(MRM)的扫描方式下正负离子同时监测,离子源为ESI源.结果:标准曲线的相关系数均高于0.9988;日内精密度和日间精密度(RSD)分别小于4.14%和4.87%;回收率在94.3% ~106.9%之间.被分析成分48 h内稳定性良好.结论:建立并验证了运用高效液相色谱-串联质谱法同时测定血塞通注射液中人参皂苷Rg1、 人参皂苷Rb1、 人参皂苷Re、 人参皂苷R、 三七皂苷R1的定性定量方法,该方法已成功地应用于云南地产的9批次的血塞通注射液中人参皂苷Rg1、 人参皂苷Rb1、 人参皂苷Rd、 人参皂苷Re、 三七皂苷R1的定性和定量分析.
Objective To develop and validate a sensitive LC-MS/MS method for the determination of Ginsenoside Rg1,Ginsenoside Rb1,Ginsenoside Rd,Ginsenoside Re and Notoginsenoside R1 in“XueSaiTong”injection,and provide theoretical basis for the improvement of the quality of“XueSaiTong”injection.Methods The chromatographic separation was performed on a CAPCELL CORE C18 column(2.1 mm×150 mm,2.7μm).The column temperature was kept at 30℃.The mobile phase was consisted of A(water)and B(acetonitrile)and the gradient elution as following:0.01~3.00min,A-B(95∶5,v/v);3.00~4.00 min,linear changed from A-B(95∶5,v/v)to A-B(30∶70,v/v);4.00~10.00 min,isocratic elution A-B(30∶70,v/v);10.00~12.00 min,linear changed from A-B(30∶70,v/v)to A-B(95∶5,v/v);12.00~15.00 min,isocratic elution A-B(95∶5,v/v).The liquid flow-rate was set at 0.300 mL/min.Multiple-reaction monitoring(MRM)was employed in both positivemode and negative mode at the same time in a single analysis process.The type of ion-source was Electron spray ionization(ESI).Result The correlation coefficient of each calibration curves was higher than 0.9988.For the precision,the overall intra-day and inter-day precisions(RSD)were obtained less than 4.14%of intra-day and 4.87%of inter-day.The average recovery was in the range of 94.3%~106.9%.The five saponins were also demonstrated to be stable within 48 h.Conclusion A sensitive LC-MS/MS method for the determination of Ginsenoside Rg1,Ginsenoside Rb1,Ginsenoside Rd,Ginsenoside Re and Notoginsenoside R1 in“XueSai-Tong”injection has been developed and validated.The proposed method was successfully appliedforthe qualitative and quantitativeanalysis of Ginsenoside Rg1,Ginsenoside Rb1,Ginsenoside Rd,Ginsenoside Re and Notoginsenoside R1 in 9 batches of“XueSaiTong”injections from different manufacturers of Yunnan province.
作者
杨崇仪
吴凡
张红宇
王莉
王玮
YANG Chongyi;WU Fan;WANG Li;WANG Wei;ZHANG Hongyu(Yunnan institute for food and drug control,Kunming 650011,China)
出处
《中国民族民间医药》
2019年第13期34-43,共10页
Chinese Journal of Ethnomedicine and Ethnopharmacy
关键词
血塞通注射液
高效液相色谱-串联质谱法
人参皂苷
三七皂苷
“XueSaiTong”Injection
Iiquid Chromatography-tandem Mass Spectrometry
Ginsenoside
Notoginsenoside
作者简介
杨崇仪(1986-),男,白族,硕士,主管药师,研究方向为药物安全性评价及药物体内动力学研究,E-mail:chongyi2002@sina.com
