Simultaneous Determination of 30 Compounds Illegally Added in Chinese Patent Medicine for Promoting Blood Circulation and Removing Blood Stasis Medicine by UHPLC-MS/MS
10.13748/j.cnki.issn1007-7693.20222257
- VernacularTitle:UHPLC-MS/MS同时测定活血化瘀类中成药中非法添加的30个化学药物
- Author:
Linlin ZHANG
1
;
Zheng LI
1
;
Huan YANG
1
;
Cheng ZHENG
1
;
Dengfeng TANG
1
;
Bilian CHEN
1
Author Information
1. Zhejiang Institute for Food and Drug Control, NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine, Hangzhou 310052, China
- Publication Type:Journal Article
- Keywords:
promoting blood circulation and removing blood stasis;
Shujin Huoxue tablets;
illegally added;
antianginal drugs;
anticoagulant;
anti-platelet aggregators;
anti-inflammatory analgesics;
UHPLC-MS/MS
- From:
Chinese Journal of Modern Applied Pharmacy
2024;41(3):359-365
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE :To establish an ultra-performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 30 compounds(including antianginal drugs, anticoagulant, anti-platelet aggregators and anti-inflammatory analgesics) illegally added in Chinese patent medicine for promoting blood circulation and removing blood stasis.
METHODS
The sample was extracted by ultrasonication with 60% methanol. The analysis was performed on Phenomenex Kinetex C18 column (2.1 mm×100 mm, 2.6 μm) with gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phase at the flow rate of 0.3 mL·min–1, and the column temperature was 40 ℃. Mass spectrometry was collected using electrospray ionization (ESI), simultaneous scanning of positive and negative ions, and multiple reaction monitoring mode.
RESULTS
The linearity of the 30 compounds was good in the mass range examined, with the correlation coefficients all >0.999. The limits of detection of each compound ranged from 1.3 to 238.4 ng·g–1 and the average recoveries ranged from 63.7% to 108.2% with the RSDs of 1.0% to 6.7%. The method was used to test 90 batches of Shujin Huoxue tablets. Paracetamol was detected in 3 batches, while the rest of the compounds were not detected. The amount of paracetamol detected ranged from 0.16 to 0.93 μg per tablet, which was much lower than the minimum daily dose of the corresponding drug, excluding intentional addition. The probable explanation was the residues caused by incomplete cleaning validation of the enterprise’s collinear production.
CONCLUSION
This method is rapid, accurate, highly sensitive, and highly selective, and can be used for qualitative screening and quantitative determination of 30 chemical compounds illegally added in Chinese patent medicine for promoting blood circulation and removing blood stasis.
