Identification of tortoiseshell glue and antler glue in Qixiong zuogui granules and content determination of 12 chemical components
- VernacularTitle:芪芎左归颗粒中龟甲胶、鹿角胶的鉴别及12种化学成分的含量测定
- Author:
Mengxiao JIA
1
;
Chunhui CHANG
1
;
Yang LIU
1
;
Yaqian WANG
1
;
Yunke ZHANG
2
;
Yongyan JIA
1
Author Information
1. College of Pharmacy，Henan University of Chinese Medicine，Zhengzhou 450046，China
2. School of Rehabilitation Medicine，Henan University of Chinese Medicine，Zhengzhou 450046，China
- Publication Type:Journal Article
- Keywords:
Qixiong zuogui granule;
tortoiseshell glue;
antler glue;
content determination;
LC-MS/MS
- From:
China Pharmacy
2025;36(5):540-545
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE To identify tortoiseshell glue and antler glue in Qichong zuogui granules， and determine the contents of 12 chemical components. METHODS Identification and content determination were performed by using liquid chromatography- tandem mass spectrometry （LC-MS/MS） method. The identification was performed on Hypersil GOLD column with a mobile phase consisted of acetonitrile-0.1% formic acid solution （gradient elution）； the electrospray ion source was used to scan in the positive ion multi-reaction detection mode. The mass charge ratio （m/z） 631.3→546.4， 631.3→921.4 was the detection ion pair for tortoiseshell glue， and the m/z 765.4→554.0， 765.4→733.0 was the detection ion pair for antler glue. The determination method for 12 chemical components was as follows： Accucore C18 column， methanol-0.1% formic acid as mobile phase （gradient elution）； scanning range of positive and negative ions was m/z 100→1 000 with the electric spray ion source and single ion detection scanning mode. RESULTS Average retention times of the molecular ion peaks for characteristic peptide segments of tortoiseshell glue and antler glue were 6.28 and 6.77 min， respectively； the linear relationship of 12 chemical components was good within their respective concentration ranges， such as astragaloside Ⅳ， calycosin-7-O-β-D-glucoside， calycosin， chlorogenic acid， ferulic acid， betaine， amygdalin， rutin， hydroxysafflor yellow A， hyperoside， loganin， cyasterone （r＞0.999）； RSDs for precision， stability （24 h） and reproducibility tests were all less than 5%. The average sample recovery rates ranged from 98.04% to 101.08%. The average contents of 12 components were 1.83， 25.73， 13.76，56.71， 23.80， 49.82， 807.49， 15.01， 317.02， 60.21， 202.71 and 17.70 μg/g， respectively. CONCLUSIONS In this study， tortoiseshell glue and antler glue in Qixiong zuogui granules are identified， and the contents of 12 chemical components therein are determined. This provides a reference for the quality control of this granule.
