TY - JOUR
T1 - Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry
AU - Lee, Hyounyoung
AU - Lim, Heungyoul
AU - Yang, Juhong
AU - Hong, Jongki
PY - 2013/12/20
Y1 - 2013/12/20
N2 - In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 (4.6 × 150 mm, 5 μm) and a Cadenza 5CD C18 column (4.6 × 150 mm, 3 μm). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity (r2 > 0.9993) within the tested ranges. The LODs and LOQs were all lower than 0.04 μg/mL. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.
AB - In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 (4.6 × 150 mm, 5 μm) and a Cadenza 5CD C18 column (4.6 × 150 mm, 3 μm). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity (r2 > 0.9993) within the tested ranges. The LODs and LOQs were all lower than 0.04 μg/mL. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.
KW - Column switching HPLC-DAD
KW - Ginkgo biloba
KW - Ginkgolic acid
KW - LC-MS/MS
KW - Method validation
UR - http://www.scopus.com/inward/record.url?scp=84891355086&partnerID=8YFLogxK
U2 - 10.5012/bkcs.2013.34.12.3629
DO - 10.5012/bkcs.2013.34.12.3629
M3 - Article
AN - SCOPUS:84891355086
SN - 0253-2964
VL - 34
SP - 3629
EP - 3634
JO - Bulletin of the Korean Chemical Society
JF - Bulletin of the Korean Chemical Society
IS - 12
ER -