摘要
目的建立中药复方制剂参苓白术散的GC指纹图谱检测方法。方法采用DB^(-1)毛细管色谱柱(30 mm×0. 32 mm,0. 5μm),载气为高纯氮气,流量为5 m L·min^(-1),检测器为氢火焰离子检测器(FID),检测器温度为290℃,气化室温度为280℃,分流比为10∶1,程序升温,进样量为1. 0μL,以正十八烷作为内参照峰,对其进行方法学验证。建立10批药材的指纹图谱共有峰。结果精密度试验各主峰相对保留时间的RSD (n=6)为0. 006%～0. 149%,相对峰面积的RSD(n=6)为0. 125%～3. 628%;重复性试验的相对保留时间的RSD(n=6)为0. 237%～0. 592%,相对峰面积的RSD(n=6)为0. 409%～3. 070%;稳定性试验的相对保留时间的RSD(n=6)为0. 031%～0. 287%,相对峰面积的RSD(n=6)为0. 144%～4. 356%。建立了10批药材的指纹图谱共有峰,各成分的相似度均大于0. 903。结论所建立的参苓白术散GC指纹图谱精密度、重复性和稳定性均符合要求,可为参苓白术散的整体质量控制提供依据。
Objective To establish a GC fingerprinting method for Shenqi Baizhu Pow der. Methods The DB-1 capillary column( 30 mm × 0. 32 mm,0. 5 μm) was used,the carrier gas was high purity nitrogen,the flow rate was 5 mL·min-1,the detector was FID,the detector temperature was 290 ℃,and the vaporization chamber temperature was at 280 ℃,the split ratio was 10: 1,the program temperature was increased,the injection volume was 1. 0 μL,and n-octadecane was used as an internal reference peak. Ten peaks of fingerprints were established for the common medicinal herbs. Results The relative retention time of each main peak in the precision test was 0. 006% to 0. 149% for RSD( n = 6),and 0. 125% for relative peak area RSD( n = 6) 3. 628%;relative retention time of RSD was 0. 237% to 0. 592% for RSD( n = 6),and RSD( n = 6) was 0. 409% to 3. 070% for relative peak area;Relative retention time of the stability test is0. 031% to 0. 287% for RSD( n = 6),and the relative peak area is RSD( n = 6) is 0. 144% to 4. 356%. A total of ten common peaks of fingerprints were established for medicinal herbs,and the similarity of each ingredient was greater than 0. 903. Conclusion The accuracy,repeatability and stability of GC fingerprints of Shenqi Baizhu Pow der are consistent with the requirements,which provides the basis for the overall quality control of Shenqi Baishu Pow der.
作者
李雪娇
李姣姣
王淼
赵旻
赵春杰
LI Xuejiao;LI Jiaojiao;WANG Miao;ZHAO Min;ZHAO Chunjie(Liaoning Electric Power Center Hospital,Shenyang 110002,China;School of Pharmacy,ShenyangPharmaceutical University,Shenyang 110016,China)
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2019年第1期61-65,共5页
Journal of Shenyang Pharmaceutical University
关键词
参苓白术散
GC指纹图谱
质量控制
Shenqi Baizhu Powder
gas chromatographic fingerprint
quality control
