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Published in: Chinese Medicine 1/2017

Open Access 01-12-2017 | Research

Quality control of Lycium chinense and Lycium barbarum cortex (Digupi) by HPLC using kukoamines as markers

Authors: Yuan-Yuan Li, Rui Di, Wing-Leung Hsu, Ye-Qing Huang, Hon-Yeung Cheung

Published in: Chinese Medicine | Issue 1/2017

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Abstract

Background

Lycii Cortex (LyC), composed of Lycium chinense and Lycium barbarum cortex and having the Chinese name Digupi, is used to treat chronic diseases like cough, hypertension, and diabetes in Eastern Asia. However, chromatographic methods, such as TLC and HPLC, to determine the phytochemical composition of LyC have not been included in any official compendiums. This study aims to establish a validated HPLC method for quality control of LyC.

Methods

Kukoamines A and B (KA and KB, respectively) were selected as markers for the HPLC method. An acetic acid solution was adopted for sample extraction because it facilitated the release of kukoamines and effectively prevented their degradation. Optimal separation of the kukoamine isomers was achieved on hydrophilic ligand-coated C18 columns with a gradient elution of acetonitrile and 0.1% (v/v) trifluoroacetic acid. The average contents and proposed contents for LyC were calculated with a t test and an uncertainty test based on 16 batches of authentic samples.

Results

The method was validated with linearity (r2 = 0.9999 for both KA and KB), precision (RSD = 1.29% for KA and 0.57% for KB), repeatability (RSD = 1.81% for KA and 0.92% for KB), and accuracy (recovery of 90.03–102.30% for KA, and 98.49–101.67% for KB), indicating that the method could offer reliable results for quality control analysis of LyC. At the 95% confidence level, the calculated content limits were 1.45 mg/g for KA and 4.72 mg/g for KB.

Conclusion

Compared with conventional morphological identification, the HPLC method involving KA and KB contents offers precise, objective, and quantitative results for quality control of LyC.
Appendix
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Literature
2.
go back to reference Yao X, Peng Y, Xu LJ. Phytochemical and biological studies of Lycium medicinal plants. Chem Biodivers. 2011;8:976–1010.CrossRefPubMed Yao X, Peng Y, Xu LJ. Phytochemical and biological studies of Lycium medicinal plants. Chem Biodivers. 2011;8:976–1010.CrossRefPubMed
3.
go back to reference Potterat O. Goji (Lycium barbarum and L. chinese): phytochemistry, pharmacology and safety in the perspective of traditional uses and recent popularity. Planta Med. 2010;76:7–19.CrossRefPubMed Potterat O. Goji (Lycium barbarum and L. chinese): phytochemistry, pharmacology and safety in the perspective of traditional uses and recent popularity. Planta Med. 2010;76:7–19.CrossRefPubMed
4.
go back to reference Committee of National Pharmacopoeia. Pharmacopoeia of the People’s Republic of China. Beijing: Chemical Industry Press; 2010. p. 115. Committee of National Pharmacopoeia. Pharmacopoeia of the People’s Republic of China. Beijing: Chemical Industry Press; 2010. p. 115.
5.
go back to reference Ministry of Health. Labor and welfare: The Japanese pharmacopoeia. Tokyo: Pharmaceuticals and Medical Devices Agency; 2012. p. 1686. Ministry of Health. Labor and welfare: The Japanese pharmacopoeia. Tokyo: Pharmaceuticals and Medical Devices Agency; 2012. p. 1686.
6.
go back to reference Korea Food and Drug Administration. The Korean herbal pharmacopoeia. Seoul: Ministry of health family welfare of South Korea; 2007. p. 1058–9. Korea Food and Drug Administration. The Korean herbal pharmacopoeia. Seoul: Ministry of health family welfare of South Korea; 2007. p. 1058–9.
7.
go back to reference Liang XM, Jin Y, Wang YP. Qualitative and quantitative analysis in quality control of traditional Chinese medicines. J Chromatogr A. 2009;1216:2033–44.CrossRefPubMed Liang XM, Jin Y, Wang YP. Qualitative and quantitative analysis in quality control of traditional Chinese medicines. J Chromatogr A. 2009;1216:2033–44.CrossRefPubMed
8.
go back to reference Lau AJ, Woo SO, Koh HL. Analysis of saponins in raw and steamed Panax notoginseng using high-performance liquid chromatography with diode array detection. J Chromatogr A. 2003;1011:77–87.CrossRefPubMed Lau AJ, Woo SO, Koh HL. Analysis of saponins in raw and steamed Panax notoginseng using high-performance liquid chromatography with diode array detection. J Chromatogr A. 2003;1011:77–87.CrossRefPubMed
9.
go back to reference Shi Z, He J, Yao T. Simultaneous determination of cryptotanshinnone, tanshinone I and tanshinone IIA in traditional Chinese medicinal preparations containing Radix salvia miltiorrhiza by HPLC. J Pharm Biomed Anal. 2005;37:481–6.CrossRefPubMed Shi Z, He J, Yao T. Simultaneous determination of cryptotanshinnone, tanshinone I and tanshinone IIA in traditional Chinese medicinal preparations containing Radix salvia miltiorrhiza by HPLC. J Pharm Biomed Anal. 2005;37:481–6.CrossRefPubMed
10.
go back to reference Wu HF, Guo J, Chen SL. Recent developments in qualitative and quantitative analysis of photochemical constituents and their metabolites using liquid chromatography-mass spectrometry. J Pharm Biomed Anal. 2012;72:267–91.CrossRefPubMed Wu HF, Guo J, Chen SL. Recent developments in qualitative and quantitative analysis of photochemical constituents and their metabolites using liquid chromatography-mass spectrometry. J Pharm Biomed Anal. 2012;72:267–91.CrossRefPubMed
11.
go back to reference Chu QC, Fu L, Lin M. Study on bioactive ingredients in Cortex Lycii by capillary zone electrophoresis with amperometric detection. Chin J Anal Chem. 2005;33:1611–4. Chu QC, Fu L, Lin M. Study on bioactive ingredients in Cortex Lycii by capillary zone electrophoresis with amperometric detection. Chin J Anal Chem. 2005;33:1611–4.
12.
go back to reference Li K, Chen XH, Bi KS. Determination of vanillic acid in Cortex Lycii by RP-HPLC. Chin Tradit Herbal Drugs. 2005;36:446–7. Li K, Chen XH, Bi KS. Determination of vanillic acid in Cortex Lycii by RP-HPLC. Chin Tradit Herbal Drugs. 2005;36:446–7.
13.
go back to reference Li K, Li Q, Yuan JS. Determination of scopoletin in Cortex Lycii by RP-HPLC. Chin Pharm J. 2005;40:1741–2. Li K, Li Q, Yuan JS. Determination of scopoletin in Cortex Lycii by RP-HPLC. Chin Pharm J. 2005;40:1741–2.
14.
go back to reference Li YY, Di R, Baibado JT. Identification of kukoamines as the novel markers for quality assessment of Lycii Cortex. Food Res Int. 2014;35:373–80.CrossRef Li YY, Di R, Baibado JT. Identification of kukoamines as the novel markers for quality assessment of Lycii Cortex. Food Res Int. 2014;35:373–80.CrossRef
15.
go back to reference Zhang JX, Guan SH, Yang M. Simultaneous determination of 24 constituents in Cortex Lycii using high-performance liquid chromatography-triple quadrupole mass spectrometry. J Pharm Biomed Anal. 2013;77:63–70.CrossRefPubMed Zhang JX, Guan SH, Yang M. Simultaneous determination of 24 constituents in Cortex Lycii using high-performance liquid chromatography-triple quadrupole mass spectrometry. J Pharm Biomed Anal. 2013;77:63–70.CrossRefPubMed
16.
go back to reference Cheung HY, Li YY, Di R, Process for isolating kukoamine. USP 9012687B2. Cheung HY, Li YY, Di R, Process for isolating kukoamine. USP 9012687B2.
17.
go back to reference US Environmental Protection Agency. Technique support document for the assessment of detection and quantitation approaches. EPA-821-R-03-005, Washington D.C. 2003. US Environmental Protection Agency. Technique support document for the assessment of detection and quantitation approaches. EPA-821-R-03-005, Washington D.C. 2003.
18.
go back to reference ICH, H. T. G. Validation of Analytical Procedure: Methodology (Q2B). International conference on harmonization. USA; 1997. ICH, H. T. G. Validation of Analytical Procedure: Methodology (Q2B). International conference on harmonization. USA; 1997.
19.
go back to reference International Organization for the Standardization: ISO/IEC Guide 98-3 uncertainty of measurement—part 3: guide to the expression of uncertainty in measurement (GUM: 1995). Geneva; 2008. International Organization for the Standardization: ISO/IEC Guide 98-3 uncertainty of measurement—part 3: guide to the expression of uncertainty in measurement (GUM: 1995). Geneva; 2008.
22.
go back to reference Parr A, Mellon FA, Colquhoun IJ. Dihydrocaffeoyl polyamines (kukoamine and allies) in potato (Solanum tuberosum) tuber detected during metabolite profiling. J Agr Food Chem. 2005;53:5461–6.CrossRef Parr A, Mellon FA, Colquhoun IJ. Dihydrocaffeoyl polyamines (kukoamine and allies) in potato (Solanum tuberosum) tuber detected during metabolite profiling. J Agr Food Chem. 2005;53:5461–6.CrossRef
23.
go back to reference Rogoza LN, Salakhutdinov NF, Tolstikov GA. Plant alkaloids of the polymethyleneamine series. Russ Chem Rev. 2005;74:381–96.CrossRef Rogoza LN, Salakhutdinov NF, Tolstikov GA. Plant alkaloids of the polymethyleneamine series. Russ Chem Rev. 2005;74:381–96.CrossRef
24.
go back to reference Cai B, Li J. Evaluation of trifluoroacetic acid as an ion-pair reagent in the separation of small ionizable molecules by reversed-phase liquid chromatography. Anal Chim Acta. 1999;399:249–58.CrossRef Cai B, Li J. Evaluation of trifluoroacetic acid as an ion-pair reagent in the separation of small ionizable molecules by reversed-phase liquid chromatography. Anal Chim Acta. 1999;399:249–58.CrossRef
25.
go back to reference Li YY, Wang H, Zhao C, Huang Y, Tang X, Cheung HY. Inentification and characterization of kukoamine metabolites by multiple ion monitoring triggered enhanced product ion scan method with a triple-quadruple linear ion trap mass spectrometer. J Agric Food Chem. 2015;63:10785–90.CrossRefPubMed Li YY, Wang H, Zhao C, Huang Y, Tang X, Cheung HY. Inentification and characterization of kukoamine metabolites by multiple ion monitoring triggered enhanced product ion scan method with a triple-quadruple linear ion trap mass spectrometer. J Agric Food Chem. 2015;63:10785–90.CrossRefPubMed
26.
go back to reference Sjödin M, Irebo T, Utas JE, Lind J, Merényi G, Akermark B, Hammarström L. Kinetic effects of hydrogen bonds on proton-coupled electron transfer from phenols. J Am Chem Soc. 2006;128:13076–83.CrossRefPubMed Sjödin M, Irebo T, Utas JE, Lind J, Merényi G, Akermark B, Hammarström L. Kinetic effects of hydrogen bonds on proton-coupled electron transfer from phenols. J Am Chem Soc. 2006;128:13076–83.CrossRefPubMed
27.
go back to reference Wagner H, Bauer R, Melchart D. Chromatographic fingerprint analysis of herbal medicines: thin-layer and high performance liquid chromatography of Chinese drugs (vol 1). New York: Springer; 2011. p. 509–19.CrossRef Wagner H, Bauer R, Melchart D. Chromatographic fingerprint analysis of herbal medicines: thin-layer and high performance liquid chromatography of Chinese drugs (vol 1). New York: Springer; 2011. p. 509–19.CrossRef
28.
go back to reference Yi LZ, Yuan DL, Liang YZ. Quality control and discrimination of Percarpium Citri Reticulatae and Pericarpium Citri Reticulatae Viride based on high-performance liquid chromatographic fingerprints and multivariate statistical analysis. Anal Chim Acta. 2007;588:207–15.CrossRefPubMed Yi LZ, Yuan DL, Liang YZ. Quality control and discrimination of Percarpium Citri Reticulatae and Pericarpium Citri Reticulatae Viride based on high-performance liquid chromatographic fingerprints and multivariate statistical analysis. Anal Chim Acta. 2007;588:207–15.CrossRefPubMed
29.
go back to reference Liang YZ, Xie PS, Chan K. Quality control of herbal medicines. J Chromatogr A. 2004;812:53–70. Liang YZ, Xie PS, Chan K. Quality control of herbal medicines. J Chromatogr A. 2004;812:53–70.
30.
go back to reference Zhao ZZ, Yuen JPS, Wu J. A system study on confused species of Chinese Materia Medica in the Hong Kong market. Ann Acad Med Singapore. 2006;35:764–9.PubMed Zhao ZZ, Yuen JPS, Wu J. A system study on confused species of Chinese Materia Medica in the Hong Kong market. Ann Acad Med Singapore. 2006;35:764–9.PubMed
Metadata
Title
Quality control of Lycium chinense and Lycium barbarum cortex (Digupi) by HPLC using kukoamines as markers
Authors
Yuan-Yuan Li
Rui Di
Wing-Leung Hsu
Ye-Qing Huang
Hon-Yeung Cheung
Publication date
01-12-2017
Publisher
BioMed Central
Published in
Chinese Medicine / Issue 1/2017
Electronic ISSN: 1749-8546
DOI
https://doi.org/10.1186/s13020-016-0121-x

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