• Title/Summary/Keyword: MS2

Search Result 7,251, Processing Time 0.031 seconds

Simultaneous Determination of 80 Unapproved Compounds using HPLC and LC-MS/MS in Dietary Supplements

  • Kwon, Jeongeun;Shin, Dasom;Kang, Hui-Seung;Suh, Junghyuck;Lee, Gunyoung;Lee, Eunju
    • Mass Spectrometry Letters
    • /
    • v.13 no.3
    • /
    • pp.58-83
    • /
    • 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.

A study on the determination of lead in whole blood by ICP/MS (ICP/MS에 의한 전혈 중 납의 분석방법 연구)

  • Park, Kyung Su;Kim, Sun Tae
    • Analytical Science and Technology
    • /
    • v.10 no.4
    • /
    • pp.240-245
    • /
    • 1997
  • An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass$^{208}$ isotope of lead. Lead concentrations of human whole blood were ranged of $2.50{\sim}22.8{\mu}g/dL$. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).

  • PDF

Evaluation of the inhibitory effect of Gynostemma pentaphyllum extracts on CYP450 enzyme activities using LC-MS/MS

  • Jun Sang Yu;Young Seok Ji;So Young Jo;Xiang-Lan Piao;Hye Hyun Yoo
    • Mass Spectrometry Letters
    • /
    • v.14 no.3
    • /
    • pp.116-119
    • /
    • 2023
  • Gynostemma pentaphyllum (Thunb.) Makino extract, a natural product with a history of traditional use, has gained attention for its potential health benefits. This study aimed to investigate its effects on key cytochrome P450 (CYP) enzymes using LC-MS/MS. Human liver microsomes and cDNA-expressed CYP2C8, CYP2C9, CYP2C19, and CYP3A4 supersomes were employed. Enzyme activity was assessed based on the formation of CYP-specific marker metabolites. The resulting data showed that the extract exhibited inhibitory effects on CYP2C8, CYP2C9, CYP2C19, and CYP3A4. Thus, G. pentaphyllum extract may influence the pharmacokinetics of drugs metabolized by CYP2C8, CYP2C9, CYP2C19, and CYP3A4. These findings emphasize the importance of considering potential herb-drug interactions when incorporating this extract into therapeutic regimens or dietary supplements.

Simultaneous Determination of Ultra-Trace Pesticides and Synthetic Materials in Surface Water by LC-ESI-MS/MS (하천수에서 LC-ESI-MS/MS에 의한 극미량 농약류 및 합성원료의 동시분석법)

  • Hong, Seon-Haw;Lee, Jun-Bae;Lee, Soo-Hyung;Cho, Young-Hwan;Shin, Ho-Sang
    • Journal of the Korean Chemical Society
    • /
    • v.59 no.3
    • /
    • pp.225-232
    • /
    • 2015
  • A liquid chromatography-electrospray ionization-tandem mass spectrometry method (LC-ESI-MS/MS) was used for determining seven pesticides (2,4-dichlorophenoxyacetic acid, methomyl, aldicarb, 2-methyl- 4-chlorophenoxy- acetic acid, molinate, carbaryl and carbofuran) and two synthetic materials (quinoline and bisphenol-A) in surface water. The analytes were extracted using solid-phase extraction (SPE). The eluate was concentrated by nitrogen gas. 100 microliters of 30% (v/v) methanol aqueous solution were used to dissolve the residue and an aliquot of the reconstituted solution was directly injected into LC-ESI-MS/MS after the filtration using 0.2 μm polytetrafluoroethylene (PTFE) syringe filter. Under the established condition, the calibration curves of the analytes were linear with correlation coefficients of above 0.997. The quantification limit was 0.002~0.011 μg/L and the relative standard deviations were less than 16.4%. In addition, accuracy was in the range of 84~107% and the recoveries were values between 56.2 and 98.6%. In this study, the developed method was applied to the analysis of real surface water samples.

Geographical origin discrimination of Korean variety, Angelica gigas Nakai by using TDU (Thermal Desorption Unit)-GC/MS (TDU-GC/MS를 이용한 한국품종 참당귀 국산 판별 기법)

  • Lee, Mi-Na;Kim, Yoon-Suk;Kim, Won-Il;Kim, Jeong-Gyu;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
    • /
    • v.63 no.1
    • /
    • pp.29-33
    • /
    • 2020
  • The objective of this study was to develop a fast and accurate method of variety discrimination and geographical discrimination origin of Korean angelica (Korean variety, Angelica gigas Nakai) by using TDU-GC/MS. Two peaks of decursin and decursinol, which are coumarin derivatives were identified in the range of Total Ion Chromatogram (TIC) RT 26.9-27.2 of the Korean angelica by GC/MS analysis at the time of condensation in a refrigerated condensation system after thermal desorption of sample extracts. In case of Chinese angelica (Chinese variety), ligustilide peak was detected at the RT 17.2. In order to investigate the difference of volatile components according to the geographical origin of Korean variety, the mass spectra were measured by TDU-GC/MS at the range of m/z 40-400 amu. The TIC of domestic cultivation and Chinese cultivation of the Korean variety, Angelica gigas Nakai showed the same tendency as a whole. However, in partial scans of TIC, two peaks detected at 15.54 and 16.05 of RT showed different peak patterns between Korean angelica (Korean variety) cultivated in Korea and in China. The ratio of Peak A (RT 15.54) and B (RT 16.05) was 0.0-0.2 for domestic cultivation and 0.5-2.8 for Chinese cultivation, confirming the possibility of discriminating origin by comparing the TIC peak pattern of TDU-GC/MS.

Effect of Cu-resistant Pseudomonas on growth and expression of stress-related genes of tomato plant under Cu stress (구리-오염 토양에서 토마토 식물의 생장과 스트레스-관련 유전자 발현에 미치는 구리-내성 Pseudomonas의 영향)

  • Kim, Min-Ju;Song, Hong-Gyu
    • Korean Journal of Microbiology
    • /
    • v.53 no.4
    • /
    • pp.257-264
    • /
    • 2017
  • Pseudomonas veronii MS1 and P. migulae MS2 have several mechanisms of copper resistance and plant growth promoting capability, and also can alleviate abiotic stress in plant by hydrolysis of a precursor of stress ethylene, 1-aminocyclopropane-1-carboxylic acid (ACC) by ACC deaminase. In 4-week pot test for tomato growth in soil contained 700 mg/kg Cu, inoculation of MS1 and MS2 significantly increased root and shoot lengths, wet weight and dry weight of tomato plants compared to those of uninoculated control. The inoculated tomato plants contained less amounts of proline that can protect plants from abiotic stress, and malondialdehyde, an oxidative stress marker than those of control. ACC synthase genes, ACS4 and ACS6, and ACC oxidase genes, ACO1 and ACO4, both involved in ethylene synthesis, were strongly expressed in Cu stressed tomato, whereas significantly reduced in tomato inoculated with MS1 and MS2. Also, a gene encoding a metal binding protein metallothionein, MT2 showed similar expression pattern with above genes. All these results indicated that these rhizobacteria could confer Cu resistance to tomato plant under Cu stress and allowed a lower level of Cu stress and growth promotion.

Change of Contrast Sensitivity Induced by Tinted Spectacle Lens (칼라필터 렌즈에 따른 대비감도의 변화)

  • Seo, Jae-Myoung
    • Journal of Korean Ophthalmic Optics Society
    • /
    • v.21 no.1
    • /
    • pp.47-51
    • /
    • 2016
  • Purpose: The purpose of this study was to investigate the change of contrast sensitivity by prescribing tinted lenses and to provide the clinical manual. Methods: Contrast sensitivity was measured for twenty adults with normal vision while they wore yellow, orange and green tinted lenses. To measure contrast sensitivity, the 5 spatial frequencies (2, 4, 6, 8 and 10 cpd) were used for 33 ms and 233 ms, respectively. Results: The contrast sensitivity was overall higher with 233 ms than 33 ms (p<0.05). The peaks of contrast sensitivity with 33 ms and 233 ms were 1.75 log unit with the yellow lens and 1. 85 log unit without the color respectively. However, there was no significance between the yellow and orange tinted lens (p>0.64) Conclusions: Yellowish tinted lens that reduces chromatic aberration and the scattering is prescribed for the various purposes to improve visual functions. Before prescribing tinted lens, identifying characteristic of user and tinted lens for cut off wavelengths is recommended.

Studies on Breeding of $F_1$ Hybrid Rice Using the Korean Cytoplasmic and Genetic Male Sterile Rice II. Breeding of Genetic Male Sterile Rices Having Backgrounds of Korean Cultivars by Transferring the Male Sterility Gene of IR36ms (세포질적 유전자적 웅성불임을 이용한 벼 일대잡종 육성연구 II. 수도 IR36ms의 웅성불임 유전자 이전에 의한 한국 수도품종의 웅성불임 계통 육성)

  • Hak-Soo SUH
    • KOREAN JOURNAL OF CROP SCIENCE
    • /
    • v.31 no.1
    • /
    • pp.74-77
    • /
    • 1986
  • The male sterility gene of IR36ms was transferred to four Korean rice cultivars Gayabyeo, Nampungbyeo Sinkwangbyeo and Suweon 296 by five times back crosses. From the BC$_4$F$_2$, the genetic male sterile rices having the backgrounds of the Krean cultivars, Gayabyeo ms, Nampungbyeo ms, Sinkwangbyeo ms and Suweon 296 ms were selected. No differences in number of panicles per hill, number of florets per panicle, heading date and length of panicle, were found between the male sterile lines and their parental cultivars in the four series of male sterile rices. The culm length of the male sterile lines was shorter than that of their parental cultivars in the four male sterile rice. Significant difference in out cross rate was found from the genetic male sterile rices having different back-grounds even though they have the same male sterility gene. The out cross rates of Gayabyeo ms, Nampungbyeo ms, Sinkwangbyeo ms and Suweon 296 ms were 11.5%, 13.1 %, 1.9% and 12.7% respectively. No difference in out cross rate was found on the genetic male sterile plants planted from I 5cm to 90cm from the pollinater.

  • PDF

Development of Simultaneous Analysis for Multiple Agricultural Pesticides in Raw Milk Products using GC-MS/MS (GC-MS/MS를 이용한 원유 원료 중 농약 동시분석법 확립)

  • Young Nae Choi;Yoon ho Shin;Hwangeui Cho;Jung Bok Kim
    • Journal of Food Hygiene and Safety
    • /
    • v.38 no.6
    • /
    • pp.420-429
    • /
    • 2023
  • GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.

Effect of Feeding Chemically Treated Mustard (Brassica campestris) Straw on Rumen Fibre Degrading Enzymes in Sheep

  • Vaithiyanathan, S.;Raghuvanshi, S.K.S.;Mishra, A.S.;Tripathi, M.K.;Misra, A.K.;Prasad, R.;Jakhmola, R.C.
    • Asian-Australasian Journal of Animal Sciences
    • /
    • v.16 no.11
    • /
    • pp.1610-1613
    • /
    • 2003
  • The aim of the experiment was to study the changes in the activities of various rumen fibre degrading enzymes due to the feeding of chemically treated mustard (Brassica campestris) straw in sheep. Mustard straw (MS) (<5 cm particle size) was treated either with urea (4% (w/w), or with 2% sodium hydroxide (NaOH), or with alkaline hydrogen peroxide (2% NaOH and 1.5% hydrogen peroxide ($H_2O_2$)) and/or supplemented with 2% (w/w) urea. Seven maintenance type rations were prepared using MS (70 parts) with molasses (5 parts) and concentrate (25 parts). They were untreated MS (CMS), urea treated MS (UMS), urea supplemented MS (MSUS), alkali treated MS (AMS), alkali treated and urea supplemented MS (AMS-US), alkali $H_2O_2$ treated MS (AHMS) and alkali $H_2O_2$ treated and urea supplemented MS (AHMS-US). They were then compressed into a complete feed block with the help of block making machine. Forty two male hoggets of Malpura breed sheep were equally distributed into each treatment group and (were) offered feed and water ad libitum. At the end of 21 days of feeding trial, rumen liquor was collected through stomach tube from three animals in each group at 0 h, 4 h, 8 h, 12 h of post feeding. Results showed that the level of enzyme varied from 8.52 to 11.12, 40.85 to 50.37, 3.22 to 3.78, 2.09 to 2.77 and 31.44 to 44.24 units/100 ml SRL respectively for carboxymethyl cellulase (CMCase), $\alpha$-amylase, microcrystalline cellulase (MCCase), filter paper (FP) degrading enzyme and $\alpha$-glucosidase. Processing of MS affected the enzyme activities, in a way, that NaOH and AHP treatment significantly reduced CMCase and FP degrading enzyme. The effect of urea treatment showed an increase in the activity of MCCase and $\alpha$-glucosidase. But the supplementation of urea increased the activity of CMCase, FP degrading enzyme and $\alpha$-glucosidase. The CMCase, $\alpha$-amylase, $\alpha$-glucosidase activities were highest at 4hr whereas MCCase and FP degrading enzyme had maximum activities at 12 h post feeding Results suggested that MS might need longer time in the rumen for its effective degradation.