• Analytical Science and Technology
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• v.30 no.6
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• pp.379-389
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• 2017

In this study, we set up an analytical method that can be used for rapid and accurate determination of representative isoquinoline alkaloids in medicinal plants using UPLC-ESI-Q-TOF MS (ultra pressure liquid chromatography-electrospray ionization-quadrupole-time-of-flight mass spectrometry). The compounds were eluted on a C18 column with 0.1 % formic acid and acetonitrile, and separated with good resolution within 13 min. Each of the separated components was characterized by precursor ions (generated by ESI-Q-TOF) and fragment ions (produced by collision-induced dissociation, CID), which were used as a reliable database. We also performed method validation: analytes showed excellent linearity ($R^2$, 0.9971-0.9996), LOD (5-25 ng/mL), LOQ (17-82 ng/mL), accuracy (91.6-97.4 %) as well as intra- and inter-day precisions (RSD, 1.8-3.2 %). In the analysis of Chelidonium majus L., magnoflorine, coptisine, sanguinarine, berberine and palmatine were detected by matching retention times and characteristic fragment ion patterns of reference standards. We also confirmed that, among the quantified components, coptisine was present in the highest quantity. Furthermore, alkaloid profiling was carried out by analyzing the fragment ion patterns corresponding to peaks of unknown components. In this manner, protopine, chelidonine, stylopine, dihydroberberine, canadine, and nitidine were tentatively identified. We also proposed the molecular structure of the fragment ions that appear in the mass spectrum. Therefore, we concluded that our suggested method for the determination of major isoquinoline alkaloids by UPLC-Q-TOF can be useful not only for quality control, but also for rapid and accurate investigation of phytochemical constituents of medicinal plants.

• Korean Journal of Pharmacognosy
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• v.43 no.2
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• pp.137-146
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• 2012

Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.

• Korean Journal of Pharmacognosy
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• v.51 no.3
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• pp.217-221
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• 2020

Cirsium japonicum var. maackii (CM) has been used to treat certain medical conditions such as hemorrhage, hepatitis, and hypertension. Cirsimaritin was previously found as the major flavonoid in CM and is said to contribute to its pharmacological effects. There are currently no reports detailing the qualitative and quantitative detection of phytochemical indicators in the aerial parts of CM. Therefore, we developed a method to rapidly identify and quantify cirsimaritin in CM using HPLC/UV, and we optimized and validated this analytical method. The results showed good linearity in the concentration range tested (0.25-0.015 mg/mL, r² ≥ 0.9999), accuracy (93.9-111.3%), and precision (RSD ≤ 0.59%). The developed method can therefore be used for the rapid evaluation of cirsimaritin in CM.

• Journal of The Korean Society of Inherited Metabolic disease
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• v.15 no.3
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• pp.138-146
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• 2015

Purpose: If early diagnosis is not made, patients with metabolic disorders as homocystinemia rapidly progress to physical defect or mental retardation resulted in storage of the toxic material into the brain. Therefore, it is necessary to develop an analytical method for a rapid screening and/or correct confirmation diagnosis. Methods: The standard solution of sulfur amino acids spiked plasma was subjected to protein precipitation with methanol, and then consecutively derivatized with trimethylsilyl (TMS) and trifluoroacyl (TFA) and determined by GC-MS. The formation of TMS derivative of the hydroxyl and TFA derivative of amino functional group was performed by BSTFA and MBTFA, respectively. Selective ion monitoring (SIM) mode was used for quantification with selected specific ions. Results: A calibration curve on standard spiked pooled plasma showed a linear relationship with correlation coefficient of 0.9936-0.9992 for all compounds over the range of 0.1-300 ng. The precision and accuracy were within S.D. of 1-15% and RSD of 1-15% for intra-day assay at 2 ng/mL, 15 ng/mL and 30 ng/mL. LOD and LOQ was 0.4 ng/mL and 4 ng/mL respectively. Conclusion: A rapid analytical method was developed to quantify sulfur amino acids and methyl malonic acid, after two-step derivatization procedure with good sensitivity and specificity on human plasma. Advantages of a new method are simplicity and rapidity. The method could be useful for routine analysis, diagnosis of homocysteinemia.

• Natural Product Sciences
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• v.17 no.2
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• pp.147-159
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• 2011

A high-performance liquid chromatography-electrospray ionization-tandem mass spectrometric method was developed to determine simultaneously eight marker constituents of Forsythiae fructus, and subsequently applied it to classify its two botanical origins. The marker compounds of Forsythia suspensa were phillyrin, pinoresinol, phillygenin, lariciresinol and forsythiaside; those of F.viridissima were arctiin, arctigenin and matairesinol. Separation of the eight analytes was achieved on a phenyl-hexyl column (150${\times}$2.0 mm i.d., 3 ${\mu}M$) using gradient elution with the mobile phase: (A) 10% acetonitrile in 0.5% acetic acid, (B) 40% aqueous acetonitrile. A few fragment ions specific to the types of lignans, among the product ions generated by collisonally induced dissociation (CID) of molecular ion clusters, such as [M-H]$^-$ or [M+OAc]$^-$ were used not only for fingerprinting analysis but for the quantification of each epimer by using multiple-reaction monitoring mode. It was shown good linearity ($r^2{\geq}$ 0.9998) over the wide range of all analytes; intra- and inter-day precisions (RSD, %) were within 9.14% and the accuracy ranged from 84.3 to 115.1%. The analytical results of 40 drug samples, combined with multivariate statistical analyses - principal component analysis (PCA) and hierarchical cluster analysis (HCA) - clearly demonstrated the classification of the test samples according to their botanical origins. This method would provide a practical strategy for assessing the authenticity or quality of the herbal drug.

• Natural Product Sciences
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• v.26 no.1
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• pp.64-70
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• 2020

Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

• Journal of Korea Water Resources Association
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• v.42 no.2
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• pp.171-176
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• 2009

This study proposes an experimental formula for cumulative runoff analysis in building roof for on-site rainwater management. We can not find an appropriate method for roof runoff analysis because of its small area scale. A new runoff equation formula for rainfall depth(D) and cumulative runoff volume(V) is developed on roof runoff conditions. Reliability of the formula is verified with field experimental runoff monitoring for two years in two buildings of rainwater management system. This experimental runoff formula can root the cumulative runoff volume from roof area and rainfall depth, then develop reasonable inflow condition for rainwater retention tank design.

• Korean Journal of Food Science and Technology
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• v.44 no.2
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• pp.247-250
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• 2012

Raw milk samples (n=28) obtained from milk tanks in 3 dairy plants of different regions and commercial milks (n=100) were collected from six cities. These samples were analyzed for the level of aflatoxin $M_1$ contamination using immunoaffinity columns and high performance liquid chromatography coupled with fluorescent detectors. Confirmation of aflatoxin $M_1$ ($AFM_1$) identified in positive samples was based on the formation of the hemiacetal derivative ($AFM_{2a}$) after derivatization with trifluroacetic acid. The average concentrations of aflatoxin $M_1$ in the raw milks were 25.1 ng/kg, and those values in commercial milks were 29.8 ng/kg. The highest level of aflatoxin $M_1$ in milk was 72.7 ng/kg. These results showed that the contamination of aflatoxin $M_1$ in milks consumed in the Korea was quite low compared to the standard in Korea Food Code (aflatoxin $M_1$ 500 ng/kg).

• Journal of the Korea Academia-Industrial cooperation Society
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• v.10 no.11
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• pp.3494-3499
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• 2009

The stability of omeprazole in the aqueous solutions containing loxoprofen or Sodium bicarbonate was examined at room temperature. Loxoprofen or Sodium bicarbonate (60 mg) was added to omeprazole (600 ${\mu}g$/ml) solution to check the stability profile. Then, the solution was kept at room temperature for 80 hours. The concentration was assayed at each concentration by stability-indicating High performance liquid chromatography (HPLC) method. Aliquots of the solution were withdrawn at specified time intervals and assayed by chromatographic analysis for intact omeprazole. The relation between omeprazole concentration and peak area was linear from 5 to 160 ${\mu}g$/ml. The analysis method was precise with relative standard deviation (% RSD) no greater than 3.05 %. The remaining percentage-time curves revealed that omeprazole was degraded rapidly as functions of time and temperature following pseudo first-order kinetics. In conclusion, the stability of omeprazole was significantly affected by liquid solutions mixed with alkalizer (Sodium carbonate) or the NSAIDs (loxoprofen).

• Analytical Science and Technology
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• v.23 no.6
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• pp.572-578
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• 2010

The extraction/clean-up and concentrating of pharmaceuticals from surface water were performed by HLB (Hydrophilic-Lipophilic Balanced) cartridge. The method allows for the simultaneous determination of six pharmaceuticals by HPLC/ESI(+)-MS/MS. Recoveries of the pharmaceutical were between 71.1 to 92.6% (except fenbendazole) and the overall variability of the method was below 11.2% (RSD). The calibration curves for the pharmaceuticals from blank surface water showed good linearities (above $r^2$ = 0.99) in the concentration range of 0.007~1.2 ng/mL. The limit of detection (LOD) and the limit of quantification (LOQ) were 7.2~128.7 pg/mL and 23.8~429.1 pg/mL, respectively. The present analytical method can be useful for monitoring residual pharmaceuticals in surface water and other aquatic samples. High concentrations of iopromide and fenbendazole were detected in a few samples of surface water.