Rapid quantification of constituents in St. John's wort extracts by NIR spectroscopy

被引:29
作者
Rager, I [1 ]
Roos, G [1 ]
Schmidt, PC [1 ]
Kovar, KA [1 ]
机构
[1] Univ Tubingen, Inst Pharmaceut, D-72076 Tubingen, Germany
关键词
Hypericum perforatum; St. John's wort extracts; NIR spectroscopy; RP-HPLC; quantification;
D O I
10.1016/S0731-7085(01)00602-1
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A quantitative near-infrared reflectance spectroscopy (NIRS) method was established for the determination of two major constituents (hyperforin and I3,II8-biapigenin) in St. John's wort extracts. Hyperforin was chosen due to the fact that it is found in a concentration range from I to 5%, a common one for NIRS determinations. I3,II8-Biapigenin on the other hand was selected as a constituent with very low concentrations (0.1-0.7%) but an extensive chromophore that allows very precise measurements in the ultraviolet (UV) and thus exact reference values that are vital for proper NIRS calibrations. Reference measurements were performed by reversed-phase high performance liquid chromatography (HPLC), determining the constituents' content in 35 pharmaceutical dry extracts of different origins. The reference method was validated according to the ICH guideline Q2B. Using partial-least squares (PLS) regression a multivariate calibration was done for the two ingredients each (PLS1). Satisfactory calibration statistics were obtained for hyperforin with a root mean square error of calibration (RMSEC) of 0.17 and a root mean square error of prediction (RMSEP) of 0.22 at a concentration range from I to 6% in the dry extracts. Due to the very low concentrations of I3,II8-biapigenin the accuracy of prediction is somewhat lower. However, it is possible to obtain very good results and reliable prediction by dividing the concentration range at 0.35%. The study emphasizes the potential of NIRS as a rapid and highly effective alternative method to conventional quantitative analysis of plant extracts. (C) 2002 Published by Elsevier Science B.V.
引用
收藏
页码:439 / 446
页数:8
相关论文
共 20 条
[1]  
[Anonymous], STAT METHODEN WASSER
[2]  
[Anonymous], 1989, MULTIVARIATE CALIBRA
[3]   Herbal remedies - Issues in licensing and economic evaluation [J].
Ashcroft, DM ;
Po, ALW .
PHARMACOECONOMICS, 1999, 16 (04) :321-328
[4]   Effect of data preprocessing methods in near-infrared diffuse reflectance spectroscopy for the determination of the active compound in a pharmaceutical preparation [J].
Blanco, M ;
Coello, J ;
Iturriaga, H ;
Maspoch, S ;
delaPezuela, C .
APPLIED SPECTROSCOPY, 1997, 51 (02) :240-246
[5]   Identification by high-performance liquid chromatography diode array detection mass spectrometry and quantification by high-performance liquid chromatography UV absorbance detection of active constituents of Hypericum perforatum [J].
Brolis, M ;
Gabetta, B ;
Fuzzati, N ;
Pace, R ;
Panzeri, F ;
Peterlongo, F .
JOURNAL OF CHROMATOGRAPHY A, 1998, 825 (01) :9-16
[6]   The influence of data pre-processing in the pattern recognition of excipients near-infrared spectra [J].
Candolfi, A ;
De Maesschalck, R ;
Jouan-Rimbaud, D ;
Hailey, PA ;
Massart, DL .
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 1999, 21 (01) :115-132
[7]   Hyperforin as a possible antidepressant component of hypericum extracts [J].
Chatterjee, SS ;
Bhattacharya, SK ;
Wonnemann, M ;
Singer, A ;
Müller, WE .
LIFE SCIENCES, 1998, 63 (06) :499-510
[8]   PARTIAL LEAST-SQUARES REGRESSION - A TUTORIAL [J].
GELADI, P ;
KOWALSKI, BR .
ANALYTICA CHIMICA ACTA, 1986, 185 :1-17
[9]   PARTIAL LEAST-SQUARES METHODS FOR SPECTRAL ANALYSES .1. RELATION TO OTHER QUANTITATIVE CALIBRATION METHODS AND THE EXTRACTION OF QUALITATIVE INFORMATION [J].
HAALAND, DM ;
THOMAS, EV .
ANALYTICAL CHEMISTRY, 1988, 60 (11) :1193-1202
[10]   High-performance liquid chromatography on-line coupled to high-field NMR and mass spectrometry for structure elucidation of constituents of Hypericum perforatum L. [J].
Hansen, SH ;
Jensen, AG ;
Cornett, C ;
Bjornsdottir, I ;
Taylor, S ;
Wright, B ;
Wilson, ID .
ANALYTICAL CHEMISTRY, 1999, 71 (22) :5235-5241