• Food Science of Animal Resources
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• v.41 no.5
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• pp.816-825
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• 2021

This study aims to validate a fast method of simultaneous analysis of 365 LCamenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 ㎍/kg), and good recoveries (70%-120%) and relative standard deviations (RSDs) (≤20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were ≤10 ㎍/kg for 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.

• Mass Spectrometry Letters
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• v.4 no.4
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• pp.79-82
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• 2013

Various types of alkaloids observed in several herbal medicines were analyzed by electrospray ionization tandem mass spectrometry in positive ion mode. In the present study, MS/MS spectralpatterns were investigated for eight-types of alkaloids (aporpine, protoberberine, tetrahydroprotoberberine, benzylisoquinoline, protopine, phthalide, morpine, and bisbenzylisoquinoline). For aporpine- and protoberberine-type alkaloids, main fragmentations occurred at substituted groups on rigid ring structures, not showing ring fusion. Interesting fragmentations due to iminolization and retro-Diels-Alder (RDA) reaction were observed in MS/MS spectra of protopine- and tetrahydroprotobereberine-type alkaloids. Also, several types of fragmentations such as inductive cleavage and ${\alpha}$-cleavage, or bond cleavage between two ring structures were observed depending on their structural characteristics. These fragmentation patterns are expected to allow instant classification of the specific alkaloid type in various MS/MS spectra of alkaloids.

• KSBB Journal
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• v.22 no.4
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• pp.234-238
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• 2007

We used electrospary ionization ion trap tandem mass spectrometry (ESI-IT tandem MS) to structural elucidation of three different biantennary-type glycans having zero, one, two galactoses (G0, G1, G2). The highest fragment ion in the MS/MS spectra of three glycans was produced by 0,2-ring cleavage of fucose-linked N-acetylglucosamine (GlcNAc) in reducing end. The fragment ions both from precursor ions and 0,2-ring cleaved ions ($^{0.2}An$; n=5 for G0, n=6 for G1 and G2) were not overlapped each other. As results of $MS^n$ analyses, tandem fragmentation trees of each glycans were generated and 2,4-ring cleavages ($^{2.4}A_6$) were occurred in GlcNAc linked to reducing end GlcNAc. This structural elucidation and fragmentation study of N-linked glycans by tandem mass spectrometry can be applied to structural analysis of more complicated glycans.

• Food Science and Biotechnology
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• v.17 no.3
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• pp.508-513
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• 2008

Erythromycin has been used to treat Streptococosis, Edwardsiel1osis, Vibriosis, Bacterial enteritis in the cultured fish. In this study, a rapid and effective erythromycin analysis method with new sample treatment protocol and liquid chromatography/tandem mass spectrometry (LC/MS/MS) system for fish products was developed. For the erythromycin extraction from fish muscle, the solvent mixture composed of 0.2% meta-phosphoric acid and methanol (6:4) showed good recovery rate, and the optimum extraction solvent volume was 20 mL. Erythromycin detection using LC/MS/MS were carried out under electro spray ionization (ESI) positive condition and erythromycin mass value 576.2 and 157.9. And the detection limit of the established method was 0.005 mg/kg in fish products. The recovery rate of the developed method applied to the fish species were as following, olive flounder, $87.6{\pm}5.0%$; black rockfish, $87.2{\pm}6.4%$; eel, $85.2{\pm}4.8%$; and rainbow trout, $86.0{\pm}6.2%$. In the established method in this study, the correlation of coefficient values ($R^2$) of erythromycin calibration curve (n=11) was 0.9998.

• Journal of Environmental Science International
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• v.24 no.12
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• pp.1569-1582
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• 2015

The analytical method for 16 organophosphorus pesticides was developed in this study. The 16 organophosphorus pesticides were analyzed by liquid chromatography-tandem mass spectrometry (LC/MS/MS) using on-line solid phase extraction (on-line SPE) with PLRP- S cartridge. Analysis of all analytes in the MS/MS was processed in the electrospray ioni-zation (ESI) positive mode. They are Azinphos ethyl, Chlorfenvinphos, Ethion, Famphur, Phosmet, Phosphamidon, Terbufos, Aspon, Chlorpyrifos-methyl, Crotoxyphos, Dichlofenthi-on, Dicrotophos, Fonofos, Thionazin, Dimethoate and Iprobenfos. Limits of detection (LODs) and Limits of quantification(LOQs) were obtained as 0.8~2.0 ng/L and 2.6~6.4 ng/L, respectively. All compounds were not detected at the 8 sampling points of the raw water and clean water.

• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1097-1102
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• 2002

The mass spectrometry using an ion trap tandem mass spectrometer has been investigated to find optimum conditions for the analysis of benzo(a)pyrene (3,4-benzpyrene). The applicability to a real soil sample was also investigated to verify the usef ulness of the MS/MS (or collision induced dissociation, CID) analysis. The optimum CID condition was 1.5 and 0.45 for the RF excitation voltage and the q value, respectively. For comparison, CID and EI were applied to the analysis of a soil sample. CID analysis was more sensitive than EI analysis of the soil sample. The limit of detection (LOD) of benzo(a)pyrene was 3.18 ng mL-1 and 0.85 ng mL,-1 for EI and MS/MS analysis, respectively. The precision at the soil sample for EI and CID showed relative standard deviations of 6.1% and 4.1%, respectively, and the concentrations were 168 ㎍ kg-1 and 162 ㎍ kg-1 , respectively.

• Mass Spectrometry Letters
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• v.9 no.1
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• pp.17-23
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• 2018

Studies on the interactions of amyloidogenic proteins with trace metals, such as copper, have indicated that the metal ions perform a critical function in the early oligomerization process. Herein, we investigate the effects of Cu(II) ions on the active sequence regions of amyloidogenic proteins using electrospray ionization mass spectrometry (ESI-MS) and collision induced dissociation tandem MS (CID-MS/MS). We chose three amyloidogenic peptides NNQQNY, LYQLEN, and VQIVYK from yeast prion like protein Sup35, insulin chain A, and tau protein, respectively. [Cu-peptide] complexes for all three peptides were observed in the mass spectra. The mass spectra also show that increasing Cu(II) concentrations decrease the population of existing peptide oligomers. The tandem mass spectrum of NNQQNY shows preferential binding for the N-terminal region. All three peptides are likely to appear to be in a Cu-monomer-monomer (Cu-M-M) structure instead of a monomer-Cu-monomer (M-Cu-M) structure.

• Analytical Science and Technology
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• v.28 no.5
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• pp.317-322
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• 2015

Simultaneous analytical method has developed for the determination of anion biocides in soil by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chlorite and chlorate in soil were extracted with pure water, and cyanuric acid and sodium dodecylbenzenesulfonate (Na-DBS) were extracted with mobile phase (0.25 mM ammonium formate in 20 mM formic acid : acetonitrile (1:1)). The extract was injected into the LC-MS/MS system after filtration. The method detection limits in this study were 0.04 mg/kg for chlorite, 0.04 mg/kg for chlorate, 0.27 mg/kg for cyanuric acid, and 0.05 mg/kg for Na-DBS, respectively. The method was applied to the analysis of 50 soil samples collected from 40 sites sprayed with biocides and 10 background sites. As a result, anion biocides were not detected in all sites.

• The Korean Journal of Pesticide Science
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• v.2 no.3
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• pp.79-84
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• 1998

Tandem HPLC and atmospheric pressure chemical ionization(APcI) LC/MS method was used for the determination and confirmation of carbendazim residues in soybean sprout. Fluorescence(FL) detector was connected in tandem with the ultraviolet(UV) detector for dual detection of the carbendazim residue at the excitation and emission wavelength of 280 nm and 310 nm, respectively. The limit of detection for carbendazim was $0.1{\mu}g/kg$ sample. Recoveries of carbendazim from fortified soybean sprout at 0.5, 1.0 and 2.0 ppm were averaged 89.1%. Mass spectrometry using a APcI source confirmed the carbendazim residue in the soybean sprout sample. Fragmentation pattern on the APcI LC/MS spectrum of carbendazim was simpler than that from electron impact(EI) mass spectrum. Carbendazim produced 3 major ions including m/z 133, m/z 159 and m/z 191($M^{+}$). This method was sensitive enough to provide reliable and reproducible results for practical applications.

• Mass Spectrometry Letters
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• v.14 no.4
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• pp.141-146
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• 2023

Liraglutide is a medication prescribed for the management of type 2 diabetes and chronic obesity. A simple, sensitive, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitative analysis of liraglutide in rat plasma. After a simple protein precipitation step, liraglutide was chromatographically separated using the ACQUITY Premier Peptide BEH C18 Column with mobile phases comprising 50% acetonitrile and 50% methanol, and water with 0.3% FA. Positive ion electrospray ionization in multiple reaction monitoring mode was used to achieve detection. Good linearity was observed in the 5-600 ng/mL concentration range (R² > 0.99). Liraglutide had intra- and inter-day precision values of 2.13%-9.86% and 4.14%-8.36%, respectively. The accuracy ranged from -2.36% to 2.58%. The recovery and matrix effect were within acceptable limits. This selective LC-MS/MS method was used to study the pharmacokinetic properties of liraglutide after subcutaneous administration in rats.