Establishment of the detection method for the adulteration of Bupleurum marginatum in Ganmao qingre granules and determination of adulteration limit
- VernacularTitle:感冒清热颗粒中藏柴胡掺伪检测方法的建立及掺伪限度拟定
- Author:
Dantong ZHAO
1
,
2
;
Yijun GAO
3
;
Tianchen BI
1
;
Jinghua LIU
1
;
Weikun ZHU
1
;
Suxiang WANG
1
;
Rong RONG
2
Author Information
1. Heze Institute for Food and Drug Control,Shandong Heze 274000,China
2. College of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250355,China
3. Dept. of Pharmacy,Heze Municipal Hospital,Shandong Heze 274031,China
- Publication Type:Journal Article
- Keywords:
Ganmao qingre granules;
Bupleurum marginatum;
nepasaikosaponin K;
adulteration;
HPLC-MS/MS
- From:
China Pharmacy
2022;33(20):2454-2459
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE To establish the de tection method for the adulteration of Bupleurum marginatum in Ganmao qingre granules,and to determine the adulteration limit . METHODS HPLC-MS/MS method was used to detect the content of nepasaikosaponin K in commercial and self -made samples of Ganmao qingre granules ,using electrospray ionization ,and the analysis was carried out under multiple reaction monitoring model in negative mode with m/z 943.6→635.5 as the quantitative ion pair. The calculation method was established for the adulteration proportion of B. marginatum in Ganmao qingre granules . Taking nepasaikosaponin K as the index ,the adulteration limit was determined . RESULTS The linear range of nepasaikosaponin K were 0.051-20.200 μg/mL(r=0.999 1). RSDs of precision ,repeatability and stability (24 h)tests were all lower than 2.50%. The average recoveries were 97.58%(RSD=2.09%,n=9). The limit of detection was 0.60 μg/g,the limit of quantitation was 1.80 μg/g. The adulteration ratio of B. marginatum in Ganmao qingre granules had a good linear relationship to the peak area of nepasaikosaponin K in the range of 5%-100%(r=0.990 9). The contents of nepasaikosaponin K in 15 batches of Ganmao qingre granules were 2.584-56.661 μg/g. One batch of samples exceeded the proposed adulteration limit (10%),and the unqualified rate was 6.67%. CONCLUSIONS The established analytical method can be used to detect the adulteration of B. marginatum in Ganmao qinggre granules ,the proposed adulteration limit is 10%.