• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3629-3634
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• 2013

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 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). 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 ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. 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.

• Analytical Science and Technology
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• v.36 no.1
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• pp.22-31
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• 2023

As the use of e-liquid cigarettes is rapidly increasing worldwide, it multiplies the potential risk undisclosed to the health of non- and smokers. To reduce the hazard, each country has its own set of regulations for controlling e-liquids. In Korea, the narrow definition of tobacco makes it difficult and have been steadily occurring tax evasion exploiting the difference in natural and artificial nicotine. Therefore, it is very important to distinguish source of nicotine for their regulation. To find biochemical discriminant markers, this study established analysis methods based on high-performance liquid chromatography coupled with diode array detector (HPLC-DAD) and high-performance liquid chromatography coupled with triple Quadrupole mass spectrometry (HPLC-MS/MS) for nicotine enantiomers and tobacco alkaloids targeted using the difference in pathways of nicotine biosynthesis and chemical synthesis. The method was validated by experimenting linearity (R² > 0.999), recovery (80.99-108.41 %), accuracy (94.11-109.73 %) and precision (0.04-8.27 %). Then, the results for discrimination of the nicotine obtained from analysis of 65 commercial e-liquid products available in Korean market was evaluated. The method successfully applied to the e-liquids and one sample labelled 'synthetic nicotine' for tax exemption was found to contain a natural nicotine product. This method can be used to determine whether an e-liquid product uses natural or artificial nicotine and monitor non-taxable e-liquid products. The method is more scientific than the existing one, which relies only on field evidence.

• YAKHAK HOEJI
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• v.55 no.5
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• pp.361-366
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• 2011

Traditional herbal medicinal preparation Bojungikki-tang (BJT) is well-known herbal medicine used as tonic. We fermented Bojungikki-tang using nine lactic acid bacteria strains and discovered two remarkably increased compositions from the fermented BJTs using HPLC/DAD analysis. HPLC/DAD-guided fractionation of the increased compositions followed by structure identification using NMR and MS identified liquiritigenin and isoliquiritigenin. These bioconversion compositions were quantitatively analyzed using HPLC-DAD. Liquiritigenin contents were highest in BJTs fermented with L. amylophilus (1.91 mg/g) and L. fermentum (1.89 mg/g), which were increased by 20-fold compared to BJT (0.09 mg/g). Isoliquiritigenin contents were highest in BJTs in fermented with L. plantarum (0.19 mg/g) and L. fermentum (0.19 mg/g), which were increased by 19-fold compared to BJT (0.01 mg/g).

• Korean Journal of Food Science and Technology
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• v.52 no.1
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• pp.26-30
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• 2020

This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R²>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

• Journal of Food Hygiene and Safety
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• v.31 no.1
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• pp.15-20
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• 2016

Malachite green was measured in 200 freshwater fish collected from local markets in Seoul using HPLC-DAD and LC-MS/MS. LC-MS/MS method was validated by linearity, accuracy, precision and limits of detection and quantification according to the CODEX's recommendation and HPLC-DAD method was applied according to the Food Code. Malachite green levels above the quantification limit of the LC-MS/MS were determined 18.5% (37) but just 1 fish was shown to contain malachite green by HPLC-DAD. Of 83 domestic fish, 21 fish were detected malachite green (25.3%). Of 117 fish from China, just 16 fish were detected malachite green (13.4%). In detection rate by species carp (35.0%), Crucian carp (30.4%), cat fish (28.0%), Korean bull head (23.8%), snake head (20.0%), eel (10.5%) and loach (7.8%) were in order. Especially, fish collected at summer were shown to contain malachite green frequently; the detection rate was 54.8%.

• Korean Journal of Medicinal Crop Science
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• v.19 no.6
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• pp.446-455
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• 2011

Galgeun-tang (GGT) is a traditional medicinal formula that is widely prescribed to treat cold, asthma, and hives in Korea. Fermented herbal medicines can be made more effective than normal herbal medicines by increasing the absorption and bioavailability of the active compounds. In this study, we fermented Galgeun-tang to produce bioconversion constituents using Lactobacillus plantarum (GGT144), and found that four peaks were decreased, three peaks were increased and two new peaks appeared in the HPLC-DAD chromatogram. After HPLC-DAD-guided fractionation of the newly-appearing compounds (1 and 5) and the increased (6, 7, and 9) compounds, the structure of the compounds was determined using NMR and MS. Using this approach the compounds were identified to be pyrogallol (1), daidzein (5), liquiritigenin (6), cinnamyl alcohol (7), and formononetin (9), respectively. In addition, the decreased compounds were identified to be daidzin (2), liquiritin (3), ononin (4), and cinnam aldehyde (8) using HPLC-DAD analysis with standard compounds. The high performance liquid chromatography method was used to quantify the nine constituents in GGT and GGT144. All calibration curves of the standard compounds displayed excellent linearity with a $R^2$ > 0.9968.

• Korean Journal of Plant Resources
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• v.31 no.6
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• pp.652-659
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• 2018

In this study, baicalin, as a marker substance of Scutellariae Radix, was quantitatively analyzed by a high performance liquid chromatography-photodiode array detector (HPLC-DAD). We identified wogonoside, baicalein, and wogonin in the Scutellariae Radix by a high performance liquid chromatography-electrospray ionization-mass spectrometer (HPLC-ESI-MS). The baicalin was separated on a Xterra C18 column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of 38% acetonitrile in 0.68% phosphoric acid. The baicalin spectrum in the Scutellariae Radix extracts was coincided by comparing with UV-visible spectrum (200-550 nm) of baicalin standard in the library. The amount of baicalin in Scutellariae Radix was 10.46%, which is higher than KFDA's guideline. The marker substances of Scutellariae Radix showed a strong base peak $[M]^+$ in the positive detection mode following as; baicalin (m/z; $271[MH^+-sugar]^+$, $447[M+H]^+$), wogonoside (m/z; $285[MH^+-sugar]^+$, $461[M+H]^+$), baicalein (m/z; $271\;[M+H]^+$), wogonin (m/z; $285[M+H]^+$). These results are consistent with the fragment pattern and molecular weight of standard components from literature.

• Journal of the Korean Society of Clothing and Textiles
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• v.38 no.1
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• pp.110-122
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• 2014

This study examined hwangbek dyeability for cotton, silk, and wool from different tree species and origin as well as their berberine and palmatine content. A total of 12 different hwangbek were examined, six purchased directly from different locations of China and six purchased from the Seoul Medicine Market. Hwangbek purchased from China were 3 Kwanhwangbek (Phellodendron amurense Rupr.) from Jilin, Liaoning, Heilongjiang and 3 Chunhwangbek (Phellodendron chinense Schneid.) from Sichuan, Yunnan, and Guangxi. Hwangbek purchased from the Seoul Medicine Market included 3 hwangbek that originated from Korea and 3 hwangbek imported from China. We extracted 2.5g of each hwangbek into 500mL of water for 60 min at $80^{\circ}C$. Dyeing was conducted using the IR dyeing machine for 30min at $55^{\circ}C$ using a 1:100 liquor ratio. Cotton was mordanted using tannic acid followed by potassium antimonyl tartrate trihydrate treatment before dyeing. Berberine and palmatine pigments in hwangbek were identified with the HPLC-DAD-MS instrument and the amount of pigment was quantified using an ion chromatogram. The results indicated that the K/S values of dyed fabrics were highly related to the amount of pigment in hwangbek used for dyeing.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.185-194
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• 2015

This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.56 no.3
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• pp.244-249
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• 2011

A sensitive and rapid high-performance liquid chromatographic-tandem mass spectrometric (HPLC/MS/MS) assay was developed for the determination of soyasaponins in soybean. Among soyasaponins, soyasaponin I was isolated and characterized from methanol extracts of soybean as analytical standards and the development of a new analytical procedure for quantification of its content in various cultivars. The structures of these compound was elucidated by $^1H$, $^{13}C$ NMR experiments and by mass spectrometric analysis. Aqueous ethanol extracts of soybean samples were injected on an Agilent XDB-C18 column ($4.6mm{\times}50mm$, $1.8{\mu}m$) with a mobile phase consisting of 10 mM ammonium acetate-acetonitrile, a flow rate of 0.3 mL/min and a total run time of 8 min. Detection was performed by mass spectrometer bin the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI) m/z at 941 ${\rightarrow}$ 615 for soyasaponin I. In the 9 soybean samples, contents of soyasaponin I ranged from 205 to 726 mg/kg, and correlated negatively with seed size.