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Original Research Article
Liquid Chromatography –
Mass Spectrometry Method for the Simultaneous
Determination and Confirmation of Seven Active
Components in Chinese Medicine Kumu Injection
Zheng-Quan Lai1,2,
Hui-Jun Liao1,2, Siu-Po
Ip2, Yu-Yang Yi1,
Shu-Jiang Shi1,
Ji-Yan Su1,3,
Xiao-Ping Lai1,3,
Zi-Ren Su1* and Zhi-Xiu Lin2*
1New Drug Research &
Development Center, Guangzhou
University of Chinese Medicine, Guangzhou, 510006,
2School of Chinese Medicine,
The
Chinese University of Hong
Kong, Shatin, N.T., Hong Kong SAR,
3Dongguan Mathematical
Engineering and Academy of Chinese Medicine, Guangzhou
University of Chinese Medicine, Dongguan, 523808, PR
China
*For correspondence: Email:
suziren@gzucm.edu.cn or
linzx@cuhk.edu.hk;
Tel:
+86 20 3935 8517，+852 3943
6347; Fax: +86 20 3935 8390，+852 2603 7203
Received: 08 October 2013
Revised accepted: 20
November 2013
Tropical
Journal of Pharmaceutical Research, January 2014; 13(1):
141-148
http://dx.doi.org/10.4314/tjpr.v13i1.20
Abstract
Purpose:
To develop and validate a
simple and selective high performance liquid
chromatography photo diode array mass spectrometry (HPLC-PDA-MS/MS)
method for simultaneous determination and confirmation
of seven major active alkaloids (6-Hydroxy-β-Carboline-1-carboxylic acid,
β-Carboline-1-carboxylic acid,
β-Carboline-1-propanoic acid,
3-Methylcanthin-5,6-dione, 4-Methoxy-3-methylcanthine-5,6-dione,
5-Hydroxy-4-methoxycanthin-6-one, 4,5-Dimethoxycanthin-6-one)
in Kumu injections (KMIs)
Methods: For the analysis of the
preparation, the optimal chromatographic condition was
achieved on a Phenomenex Gemini C18 column
with gradient elution of 25 mM aqueous ammonium acetate
(pH = 4.0 adjusted by glacial acetate acid) and
acetonitrile with flow rate at 1.0 mL/min, column
temperature at 35 oC and detection
wavelengths at 245, 260 and 271 nm.
Results:
Excellent linear behavior
over the investigated concentration ranges was observed
with regression coeffcient (R2) > 0.9997 for
all analytes. Intra- and inter-day precisions for all
studied constituents ranged from 0.20 to 1.80 %.
Recoveries of the assayed constituents were in the range
of 98.73 to 100.34 %. The results showed the contents of
these seven marker compounds differed significantly
among different batches of KMIs both from the same and
different manufacturers.
Conclusion:
The validated method was
reliable, accurate, repeatable and can be applied to
routine quality assessment of these active components in
KMIs.
Keywords:
Alkaloids, High
performance liquid chromatography, Photo diode array,
Mass spectrometry, Kumu injection, Quality
control. |
