• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.319-331
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• 2023

Aminoglycoside antibiotics, also known as aminoglycosides (AGs), are veterinary drugs effective against a wide range of gram-negative and gram-positive bacteria. Owing to their recent use in cultured meats, it has become essential to establish an analytical method for safety management. AGs are highly polar compounds, and ion-pair reagents (IPRs) are used to ensure component separation. Owing to the high possibility of potential mechanical problems resulting from IPR addition to the mobile phase, an analytical method in which IPRs are added directly to the vial was explored. In this study, methods for analyzing 10 AGs via liquid chromatography-tandem mass spectrometry (LC-MS/MS) with the addition of two IPRs were validated for selectivity, detection limit, quantitation limit, recovery, and precision. The detection limit was 0.0001-0.0038 mg/kg, the quantification limit was 0.004-0.011 mg/kg, and the linearity (R²) within the concentration range of 0.01-0.5 mg/kg was over 0.99. Recovery and precision (expressed as relative standard deviation) evaluated in the two matrices (beef and cell culture media) ranged from 70.7% to 120.6% and 0.2% to 24.7%, respectively. The validated AG analytical method was then applied to 15 meats prepared from chicken, beef, and pork, and 6 culture media and additives used in cultured meat. No AGs were detected in any of the 15 meats distributed in Korea; however, streptomycin and dihydrostreptomycin were detected at levels ranging from 695.85 to 1152.71 mg/kg and 6.35 to 11.11 mg/kg, respectively, in the culture media additives. The LC-MS/MS method coupled with direct addition of IPRs to the vial can provide useful basic data for AG analysis and safety evaluation of meats as well as culture media and additives for cultured meats.

• Analytical Science and Technology
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• v.8 no.4
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• pp.675-682
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• 1995

Thin films of buckminsterfullerene($C_{60}$) formed by solution drop casting on Pt foil electrode surfaces were studied by cyclic voltammetry(CV) in acetonitrile(MeCN) containing quaternary ammonium or alkali-metal salts as supporting electrolyte. The electrochemical behaviors of $C_{60}$ films are found to be strongly dependent on the nature of the supporting electrolytes, especially with tetrabutyl ammonium perchlorate (TBAP, $NBu_4ClO_4$), and tetrabutyl ammonium tetrafluoroborate ($TBABF_4$, $NBu_4BF_4$). Reasonably stable films are formed into which electrons can be injected. The interaction of $C_{60}$ film with the quaternary ammonium cation may produce the fulleride salts $(TBA^+)(C{_{60}}^-)$ and $(TBA^+)_2(C{_{60}}^{2-})$. The bulk electroreduction with a controlled potential to generate the soluble $C{_{60}}^{3-}$ anions(dark red-brown color) is followed by electrooxidative deposition to produce a neutral $C_{60}$ film on the surface. The peak currents($I_{pc}$ and $I_{pa}$) of these thin film were dramatically decreased with repetitive potential scanning. These results could be explained by the adsorption-desorption phenomena and ion pairing interaction of reduced species($C{_{60}}^-$, and $C{_{60}}^{2-}$) onto the electrode surface. The peak current changes and peak potential shifts of the thin $C_{60}$ film in cyclic voltammograms formed from solution were observed by varying scan rates.

• Analytical Science and Technology
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• v.22 no.4
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• pp.319-325
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• 2009

An effective and specific procedure for confirmation of neomycin, aminoglycoside antibiotic in honey was developed and validated. Honey was adjusted to pH 2 with 0.1M HCl and applied to weak cation-exchange SPE cartridge. Neomycin was eluted with basified methanol. Following separation by ion-pairing liquid chromatography, neomycin was analysed with positive electrospray ionization and MRM mode. Quantification was linear over the range of $5.0{\sim}250.0{\mu}g/kg$ ($r^2$ >0.9951). The precision (R.S.D.) and accuracy (as a bias) of quality control samples in honey ranged 11.5~18.7% and 10.9~20.9%, respectively. Established method can be applied to analysis of neomycin in honey.

• FOCUS: LIFE SCIENCE
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• no.1
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• pp.1.1-1.4
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• 2024

This article provides comprehensive guidance on the maintenance, cleaning, regeneration, and storage of silica-based HPLC (High-Performance Liquid Chromatography) columns. The general considerations emphasize the importance of using in-line filters and guard cartridges to protect columns from blockage and irreversible sample adsorption. While these measures help, contamination by strongly adsorbed sample components can still occur over time, leading to an increase in back pressure, loss of efficiency, and other issues. To maximize column lifetime, especially with UHPLC (Ultra-High Performance Liquid Chromatography) columns, it is advisable to use ultra-pure solvents, freshly prepared aqueous mobile phases, and to filter all samples, standards, and mobile phases. Additionally, an in-line filter system and sample clean-up on dirty samples are recommended. However, in cases of irreversible compound adsorption or column voiding, regeneration may not be possible. The document also provides specific recommendations for column cleaning procedures, including the flushing procedures for various types of columns such as reversed phase, unbonded silica, bonded normal phase, anion exchange, cation exchange, and size exclusion columns for proteins. The flushing procedures involve using specific solvents in a series to clean and regenerate the columns. It is emphasized that the flow rate during flushing should not exceed the specified limit for the particular column, and the last solvent used should be compatible with the mobile phase. Furthermore, the article outlines the storage conditions for silica based HPLC columns, highlighting the impact of storage conditions on the column's lifetime. It is recommended to flush all buffers, salts, and ion-pairing reagents from the column before storage. The storage solvent should ideally match the one used in the initial column test chromatogram provided by the manufacturer, and column end plugs should be fitted to prevent solvent evaporation and drying out of the packing bed.

• Korean Journal of Food Science and Technology
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• v.36 no.6
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• pp.893-899
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• 2004

Method for sample preparation and quantitative analysis of 19 permitted and non-permitted synthetic colors in foods was developed based on reversed-phase ion-pairing high performance liquid chromatography. For color extraction of samples, deionized water was added, and pH was appropriately adjusted with 1% ammonia water. Any undissolved matters were extracted with 50% ethanol or 70% methanol. Lipid in snacks was first removed using n-hexane with centrifugation, water was added to extract colors, followed by clean-up and concentration using Sep-Pak $C_{18}$ cartridge. Recovery efficiencies at known concentrations of 19 standard food colors spiked into foods were in 90.3-97.9% range far soft drink, 79.2-101.9% for candy, 84.1-103.4% for jelly, 86.4-100.8% for chewing gum, 83.5-103.4% for ice cream, and 78.5-95.6% for snack.

• Journal of Applied Biological Chemistry
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• v.53 no.1
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• pp.25-30
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• 2010

This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

• Bulletin of the Korean Chemical Society
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• v.32 no.8
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• pp.2648-2656
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• 2011

A simple HPLC-DAD method was developed and validated to determine B group vitamin content (thiamine, riboflavin, nicotinamide, pantothenic acid, pyridoxine and folic acid) in supplemented food samples, i.e., infant formula, cereal, low-calorie food, a multi-vitamin pill and a vitamin drink. In this study, the most significant advantages were simultaneous determination of the six B group vitamins in various food matrices and a small number of sample treatment steps that required only an organic solvent, acetonitrile. Moreover, this method prevents reduction of column durability, because the mobile phase does not contain ion-pairing reagents. Analytes were separated on a Develosil RPAQUEOUS $C_{30}$ (4.6 mm ${\times}$ 250 mm, 5 ${\mu}M$ particle size) column with a gradient elution of acetonitrile and 20 mM phosphate buffer (pH 3.0) at a flow rate between 0.8 and 1.0 mL/min. Detection was performed at 275 nm, except for that of pantothenic acid (205 nm). The calibration curves for all six vitamins showed good linearity with correlation coefficients ($r^2$) higher than 0.995. The developed method was validated with respect to linearity, intra- and inter-day accuracy and precision, limit of quantification (LOQ), recovery and stability. The method showed good precision and accuracy, with intra- and inter-assay coefficients of variation less than 15% at all concentrations. The recovery was carried out according to the standard addition procedure, with yields ranging from 89.8 to 104.4%. This method was successfully applied to the determination of vitamin B groups in supplemented food products.

• The Korean Journal of Mycology
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• v.39 no.3
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• pp.239-242
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• 2011

Eritadenine, a potent compound of hypocholesterolemic activity, was investigated in relation to its content in domestic cultivars and wild types of shiitake (Lentinula edodes). Eighteens strains of shiitake were tested for the quantification of eritadenine by LC-MS/MS analysis. Among the strains, wild type-40 was highest as the content was 3.912 mg/g. Also, Soohyangko was 3.352mg/g, Sanlim No. 9 3.008mg/g, Chunbaegko 2.832 mg/g, Gaeulhyang and KFRI 675 both 2.792 mg/g as high-content strains. Soohyangko and Chunbaegko are applied strains for registration in 2010. Soohyangko is high-temperature type with concentrated fruiting, and 90% of production occurs in the first year, thus, recovery of cost is very fast. Chunbaegko is mid-temperature type with concentrated flushing, and produces "hwago", the best quality, in spring. Wild type-40 is excellent in productivity and is prepared for registration. Wild type-40 could be used as parent strain to make new strain with high eritadenine content.

• Korean Journal of Food Science and Technology
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• v.50 no.1
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• pp.14-20
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• 2018

Perfluorinated compounds (PFCs) have recently been recognized as global environmental pollutants. This study was performed to develop an analytical method for determination of levels of PFCs in food by LC-MS/MS. One hundred and nine food products were divided into two groups based on their fat and protein contents (high and low), following which samples containing high fat and protein contents were pooled and subjected to pretreatment consisting of enzymatic degradation and hexane extraction. The limit of detection of 17 PFCs in the samples were in the range of 0.013-0.145 ng/g. The degrees of precision of detection for group 1 (samples with low fat and protein contents) and group 2 (samples with high fat and protein contents) were 0.8-21.1 and 1.7-28.2%, respectively, with an accuracy of 78.8-109.8% for group 1 and 80-114.5% for group 2. This study indicated that pretreatment of high fat and protein foods with enzymatic degradation and hexane extraction would improve the detection of PFCs in food.