• 생약학회지
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• 제48권4호
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• pp.320-328
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• 2017

Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.

• 분석과학
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• 제34권4호
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• pp.160-171
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• 2021

Synthetic azo dyes are used extensively in herbal medicines to render the medicines more visually attractive to consumers. This study developed and validated a rapid high-performance liquid chromatography (HPLC) method to determine whether synthetic colorants such as Tartrazine, Auramine O, Metanil yellow, Sunset yellow, and Orange II are used extensively in Typha orientalis. To increase the recovery of the synthetic dyes, this method employed containing 50 mM ammonium acetate in 70 % methanol at first extraction and 100 mM HCl in 70 % methanol at second extraction. Five synthetic pigments in Typha orientalis were separated by gradient elution with a mobile phase consisting of acetonitrile and 50 mM ammonium acetate in distilled water at ultra-violet (UV) detection 428 nm or 500 nm. Additionally, this study established the liquid chromatography tandem mass spectrometry (LC-MS/MS) method to confirm positive samples suspected by HPLC results. The HPLC-UV method had good linearity, indicating r²> 0.999. The recoveries of the samples spiked with three different concentration ranged from 73.8~91.5 %, and relative standard deviation values indicated 0.2~5.2 %. The established LC-MS/MS could successfully identify the synthetic pigments in herbal medicine samples. The study demonstrates that Typha orientalis adulterated by yellowish synthetic dyes can be successfully distinguished when using the HPLC-UV method.

• 한국식품저장유통학회지
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• 제30권2호
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• pp.235-246
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• 2023

Yellowball (Citrus hybrid cv. Yellowball ) is a new citrus hybrid between Haruka (C. tamurana × natsudaidai ) and Kiyomi (C. unshiu × sinensis) and is known to possess strong antioxidant activity. However, detailed information on the antioxidant components of its peel has not yet been reported. This study evaluated the antioxidant activity of the peel and identified the antioxidant components by fractionating a methanolic extract of Yellowball peels using liquid-liquid extraction with n-hexane, ethyl ether (ether), ethyl acetate (EA), butanol, and water. The phenolic contents and antioxidant activities of the n-hexane, ether, and EA fractions were higher than those of the other fractions, and these fractions were further separated by semi-preparative high-performance liquid chromatography (HPLC). Four antioxidant peaks, EA1, EA2, EA3, and He1, were isolated and analyzed using ultra-performance liquid chromatography-quadrupole-time- of-flight mass spectrometry (UPLC-Q-TOF MS). Sinapoyl glucoside and hesperidin were identified in EA2 and EA3, respectively, and a polymethoxylated flavone (PMF) complex (5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone, natsudaidain, tetrameth- oxyflavone, and tangeretin) was identified in He1. A compound in EA1 with m/z 223.0246 [M-H] could not be identified and was named unknown2. The antioxidant activity of unknown2 (IC₅₀=69.17 ㎍/mL) was similar to that of Trolox, which was noted as a major antioxidant in Yellowball peel. Further studies on the antioxidant capacity of Yellowball peel are required; however, these results provide a foundation for using Yellowball peel as an antioxidant.

• 농약과학회지
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• 제16권3호
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• pp.195-201
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• 2012

본 연구는 경기도에서 유통 중인 수입과실류에 대한 잔류농약 분석을 수행하였다. 총 22품목 124건의 시료를 구입하여 GC/NPD-ECD, TOF/MS, UPLC/PDA 및 HPLC/FLD, LC/MS/MS를 이용하여 218종 잔류농약을 동시 다성분 분석법으로 분석한 결과 18건의 과실에서 잔류농약이 0.003~0.3 mg/kg 범위로 검출되었으나 기준초과 시료는 없었다. 과실의 부위별 특성에 따른 잔류농약정도를 알아보기 위해 농약이 검출된 과실류 중 14건에 대하여 분리 실험을 실시하였으며, 그 결과 과피 14건에서 0.03~1.5 mg/kg, 과육의 경우 2건에서 검출한계 미만으로 나타났다. 실험결과 모두 잔류농약허용기준 이내에서 검출되어 정상적인 방법으로 섭취할 경우 위해도는 매우 낮은 수준이었다. 그러나 미량이라도 장기간 섭취시 인체에 유해할 수 있으며, 검출빈도가 높은 성분들이 검출되므로 수입과실에 대한 지속적이고 체계적인 모니터링이 필요하겠다.

• Parasites, Hosts and Diseases
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• 제55권4호
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• pp.409-416
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• 2017

The high prevalence of pediculosis capitis, commonly known as head lice (Pediculus humanus capitis) infestation, has led to the preparation of a community-based pediculicidal ointment, which is made of common household items and the extract of Tinospora crispa stem. The present study aimed to evaluate the safety, efficacy, and physicochemical characteristics of the T. crispa pediculicidal ointment. The physicochemical properties of the ointment were characterized, and safety was determined using acute dermal irritation test (OECD 404), while the efficacy was assessed using an in vitro pediculicidal assay. Furthermore, the chemical compounds present in T. crispa were identified using liquid-liquid extraction followed by ultra-performance liquid chromatography quadruple time-of-flight mass spectrometric (UPLC-qTOF/MS) analysis. The community-based ointment formulation was light yellow in color, homogeneous, smooth, with distinct aromatic odor and pH of $6.92{\pm}0.09$. It has spreadability value of $15.04{\pm}0.98g{\cdot}cm/sec$ and has thixotropic behavior. It was also found to be non-irritant, with a primary irritation index value of 0.15. Moreover, it was comparable to the pediculicidal activity of the positive control $Kwell^{(R)}$, a commercially available 1% permethrin shampoo (P>0.05), and was significantly different to the activity of the negative control ointment, a mixture of palm oil and candle wax (P<0.05). These findings suggested that the community-based T. crispa pediculicidal ointment is safe and effective, having acceptable physicochemical characteristics. Its activity can be attributed to the presence of compounds moupinamide and physalin I.

• 생약학회지
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• 제46권3호
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• pp.189-194
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• 2015

Validation and contents determination of (+)-catechin and diosgenin from Smilax china L. rhizome (SC) were confirmed using Ultra-Performance Liquid Chromatography (UPLC). (+)-Catechin was isolated from 60% prethanol SC extract and diosgenin was isolated by acid hydrolysis of saponin fraction from 60% prethanol extract of SC. Finally we have established the validation of the isolated compounds [(+)-catechin, diosgenin] and contents determinations of (+)-catechin and diosgenin by UPLC on 60% prethanol extract of SC [(+)-catechin: 0.06878%, diosgenin: 0.48169%], and on hot water extract of SC [(+)-catechin: 0.06584%, diosgenin: 0.42178%].

• 생약학회지
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• 제48권1호
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• pp.88-92
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• 2017

In the present study, we carried out quantitative analysis of chrysin and pinocembrin in Korean propolis by ultra performance liquid chromatography (UPLC) equipped with diode array detector. The separation was done using BEH C18 ($2.1{\times}50mm$, $1.7{\mu}m$) column with a mobile phase consisting of MeCN and 0.1% $H_3PO_4$ at 280 nm. The chromatographic method was validated for specificity, limit of detection, limit of quantification, linearity, precision, and accuracy. A quantitative analysis exhibited that the contents of the two compounds in Korean propolis collected from 8 inland areas except Jeju-do ranged from 3.1-46.0 mg/g. These results will be valuable as basic data for standardization of Korean propolis.

• 생약학회지
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• 제49권1호
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• pp.70-75
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• 2018

Acer tegmentosum Maxim (ATM) has been used to treat hepatic disorders in traditional oriental medicine. However, there is little information about phytochemical constituents for quality control of ATM. In this study, we developed and established a simultaneous analytical method of the 10 marker compounds (three coumarins, 3 flavonoids, 1 lignan, 3 phenolics) in ATM using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS). Chromatographic separation of ten target analytes was achieved with a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$), using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. Identifications and quantitation of all analytes were performed using a Q-Exactive UPLC-MS/MS system. Correlation coefficients of the calibration curve for all analytes were ${\geq}0.9986$. The values of limits of detection and quantification of all analytes were 0.5-10.0 and 5.0-50.0 ng/mL, respectively. The established UPLC-MS/MS method successfully identified all target analytes in ATM, and the phytochemicals were 0.01-67.98 mg/g in its lyophilized water extract.

• 분석과학
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• 제30권5호
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• pp.221-225
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• 2017

Thioctic acid is a vitamin-like antioxidant which is prepared as tablets and injection. The Korean Pharmacopoeia (KP XI) contains monograph for the quality control of raw thioctic acid using ultra-violet visible spectrophotometry and its formulations using high performance liquid chromatography (HPLC). In British Pharmacopoeia 2013 (BP2013), another HPLC method is used for the assay test of thioctic acid material. For the international harmonization, we present an HPLC method for quantitation of thioctic acid in both raw material and tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9995$), while the RSDs for intra- and inter-day precision were 0.93 ~ 1.26 % and 1.40 ~ 1.76 %, respectively. Accuracies ranged from 98.13-100.00 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.197-203
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• 2014

A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.