• Bulletin of the Korean Chemical Society
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• v.28 no.7
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• pp.1187-1194
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• 2007

The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. These methods were fully validated with respect to the linearity, accuracy, precision, recovery and robustness. The HPLC/UV method was applied successfully to the quantification of three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

• The Journal of Korean Obstetrics and Gynecology
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• v.26 no.4
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• pp.48-65
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• 2013

Objectives: We took breast milk samples and analyzed them using HPLC and LC/MS/MS, to evaluate the effects of taking Saenghwa-tang during breastfeeding on breast milk. Methods: The study participants were 20 lactating women who admitted in Korean medical postpartum care center. Breast milks were collected from paticipants who have been administrated Saenghwa-tang for more than 3 days. We used HPLC and LC/MS/MS for the determinations of amygdalin, liquiritins, 6-gingerol, decursin and decursinol angelate in Saenghwa-tang. Results: 1. Participants' $Mean{\pm}S.D$ (standard deviation) of age is $31.05{\pm}1.96$, and 15 participants had normal delivery and 5 participants had cesarean delivery. 12 participants were primipara and 8 participants were multipara. $Mean{\pm}S.D$ of lactating date is $9.4{\pm}0.94$. 2. Using HPLC, we learned LOQ level peak that matches the peak retention time of standard components of Saenghwa-tang was not detected from 20 breast milk samples. 3. Using LC/MS/MS, decursin of Angelicae Gigantis Radix was detected from HMSP 02, HMSP 04, HMSP 06, HMSP 11, and the each concentrations are 16, 2, 64, 11 ppb. Liquiritin of Glycyrrhizae Radix was not detected from HMSP 13~HMSP 18. Conclusions: Data obtained by this approach shows that this method is reliable and suitable for determining the safety of taking Saenghwa-tang during breastfeeding.

• Analytical Science and Technology
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• v.22 no.1
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• pp.65-74
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• 2009

Active components of lacquer tree referred to as urushiol congeners, which are catechol derivatives with various alkyl or alkenyl substituents. The olefin side chains typically have one, two or three double bonds. In this study, the each congener's ratio analysis of extracts from korean lacquer tree are compared to the one from other asian lacquer tree. Extraction was performed using liquid-liquid extraction (LLE) method with soxhlet system from tree's bark and sap. Extracts were analyzed by reverse phase liquid chromatography and on-line electro spray ionization mass spectrometry (LC-MS/MS).

• Journal of environmental and Sanitary engineering
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• v.21 no.1 s.59
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• pp.35-43
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• 2006

Formaldehyde is important because of their irritant and toxic properties, mutagenicity and carcinogenicity. In this study, liquid chromatography-mass spectrometry (LC-MS) is used for the analysis of formaldehyde after derivatization with 2,4-dinitrophenylhydrazine (DNPH) cartridge. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearity ($r^2$) was 0.9997 when analyte concentration ranges from 25 to $200{\mu}g/l$. The relative standard deviation (%RSD) was 1.25 % for concentration of $200{\mu}g/l$. The minimum detection limit (MDL) was 0.73 ppbv. It was shown that LC-MS method has a great potential for formaldehyde analysis. The results of formaldehyde from the survey of Ban-Woll and Shi-Hwa Industrial Complex samples, the highest level was 6.20, 3.93 ppb, respectively. The highest emission level of formaldehyde at chemical plants in the Ban-Woll' Shi-Hwa Industrial Complex was 5421.25 ppb.

• Analytical Science and Technology
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• v.15 no.6
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• pp.574-579
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• 2002

A sensitive and easy high performance liquid chromatograph (HPLC) / electrospray ionization (ESI)-mass spectrometric (MS) method has been developed for the quantitative and qualitative analyses of acarbose and its metabolites. After plasma samples were simply filtered with a syringe filter, the filtered plasma was analyzed by LC/MS. The standard calibration curve for acarbose was linear ($r^2=0.9963$) over the concentration range $0.1{\sim}10{\mu}g/m{\ell}$ in plasma. The metabolite component-I and II, which were metabolized by the ${\alpha}$-amylase and ${\beta}$-amylase, were found also by in vitro incubation. The developed method can be utilized to study acarbose and the other carbohydrates.

• Journal of Korean Society on Water Environment
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• v.25 no.5
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• pp.720-726
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• 2009

We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.

• Journal of the Korean Chemical Society
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• v.55 no.4
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• pp.626-632
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• 2011

Phoxim, which is one of veterinary drugs, is a well-known antiparasitic agent in wide use. In this paper, phoxim was extracted from cattle and pig tissue using solid-phase extraction (SPE) employing a silica cartridge with acetonitrile. Liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) for the analysis of phoxim from animal tissue was presented. Phoxim was detected on a $C_{18}$ column ($2.1{\times}100\;mm$, $3.5\;{\mu}m$) using a mobile phase of 0.1% formic acid in water and acetonitrile. A linear correlation observed in the calibration curves for cattle (0.0048~2.0 mg/kg) and pig (0.0055~2.0 mg/kg) showed above $r^2$=0.995. Accuracy measured at concentrations ranging from 0.0048 to 0.2 mg/kg was the range of 68.2~106.9%. Limit of detection (LOD) and limit of quantitation (LOQ) were the range of 0.0014~0.0017 mg/kg and 0.0048~0.0055 mg/kg, respectively. The precision (RSD%) was below 11.2%.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.54 no.4
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• pp.404-410
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• 2021

Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R²) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 ㎍/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 ㎍/kg and 0.23-0.50 ㎍/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.

• Mass Spectrometry Letters
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• v.13 no.3
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• pp.58-83
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• 2022

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL^-1; linearity (r²) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL^-1, linearity (r²) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.296-313
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• 2014

A QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) multiresidue method was developed for the simultaneous analysis of 124 pesticides in soil by LC-MS. The procedure involved liquid extraction of soil immersed with 0.2N $NH_4Cl$ by acetonitrile with 1% acetic acid, followed by anhydrous $MgSO_4$ and sodium acetate, and dispersive SPE cleanup with $MgSO_4$, primary secondary amine (PSA) and $C_{18}$. The extracts were analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.99. Recovery studies for the validation were carried out using two type soils, loam and sandy loam, at four concentration levels (0.005, 0.01, 0.02, and 0.1 mg/kg). The recoveries of pesticides were in the range of 70-120% with < 20% RSD except 4 pesticides, Benfuracarb, Ethiofencarb, Pymetrozine, and Pyrethrin. This result indicated that the method using QuEChERS and LC-MS/MS could be applied for the simultaneous determination of pesticide residues in soils.