摘要
目的:建立同时测定荆防败毒口服液中4个有效成分(升麻素苷、紫花前胡苷、二氢欧山芹醇当归酸酯和欧当归内酯A)含量的LC-ESI/MS方法。方法:通过优化,建立了如下方法同时测定荆防败毒口服液中4个有效成分(升麻素苷、紫花前胡苷、二氢欧山芹醇当归酸酯和欧当归内酯A):采用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm),柱温为30℃,以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~10 min,90%A→0%A;10~11 min,0%A→90%A;11~13 min,90%A),流速0.2 m L·min^(-1),分析时间为13 min,进样量1μL;采用ESI正负离子模式,多反应监测(MRM),应用Masslynx V4.1软件进行数据分析。结果:升麻素苷、紫花前胡苷、二氢欧山芹醇当归酸酯和欧当归内酯A能够在13 min内完全分离,质量浓度在一定范围内与峰面积呈良好的线性关系(r2>0.998),日内精密度RSD为0.19%~0.68%,日间精密度RSD为0.74%~1.9%,重复性RSD为0.11%~1.9%,稳定性RSD为3.3%~8.6%,加样回收率在97.7%~102.3%(RSD为0.50%~2.7%);测得的4批样品中升麻素苷、二氢欧山芹醇当归酸酯、紫花前胡苷和欧当归内酯A的含量范围分别为2.27~2.52、6.35~7.06、143.14~180.534和0.076~0.186μg·m L^(-1)。结论:该方法可以用于荆防败毒口服液中4个有效成分的含量测定和质量控制。
Objective： To establish a LC-ESI/MS method for （prim-O-glucosylcimifugin, nodakenin, columbianadin and The separation was performed on an ACQUITY UPLC BEH elution （ 0-10 min, 90%A →0%A; 10-11 min, 0%A → simultaneous determination of four bioactive constituents levistolide A ）in Jingfangbaidu oral liquid. Methods： Cls column（ 2. 1 mm × 50 mm, 1.7 μm ）with gradient 90%A; 11-13 min, 90%A ）using 0. 1% formic acid （ A ） and acetonitrile （ B ） as mobile phase. And the column temperature, flow rate, injection volume and analysis time were 30 ℃, 0. 2 mL·min^-1, 0. 1 μL and 13 min, respectively. Quantification of the analytes was performed on a Triple quadrupole mass spectrometer. A multiple-reaction monitoring scanning and an electrospray ionization （ ESI ） - tandem interface in the positive and negative ion polarity mode were employed. Data analysis was operated on Masslynx V4. 1 software. Results： Four ingredients, prim-O-glucosylcimifugin, nodakenin, columbianadin and levistolide A could be separated in 13 min, and all calibration curves showed good linearity （ r2〉0. 998 ）within the test range. The RSD of intra-day precision, inter-day precision, repeatability and stability were within 0. 19%-0. 68%, 0. 74%-1.9%, 0. 11%-1.9% and 3.3%-8. 6%, respectively. The average recoveries for the four analytes were between 97. 7% and 102. 3%, and the RSD was within 0. 50%-2. 7%. The contents ofprim-O-glucosylcimifu^n, nodakenin, columbianadin and levistolide A in four batches of samples were within 2.27-2.52 μg·mL^-1, 6. 35-7.06 μg·mL^-1, 143.14- 180. 534μg·mL^-1 and 0. 076-0. 186 μg·mL^-1, respectively. Conclusion： The proposed method could be used to determine the four components and quality control of Jingfangbaidu oral liquid.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第8期1489-1496,共8页
Chinese Journal of Pharmaceutical Analysis
关键词
中药制剂
荆防败毒口服液
防风
羌活
独活
川芎
升麻素苷
紫花前胡苷
二氢欧山芹醇当归酸酯
欧当归内酯A
TCM preparation
Jingfangbaidu oral liquid
Radix sileris
Notopterygium root
Angelica
Ligusticum wallichii
prim-O-glucosylcimifugin
nodakenin
columbianadin
levistolide A
