• Journal of Genetic Medicine
• /
• v.4 no.1
• /
• pp.45-52
• /
• 2007

Purpose : A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-ex tensive pre-treatment by electrospray ionization MS/ MS (ESI-MS/MS). Measurement of globotriaosy lceramide (Gb3, ceramide trihex oside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. Methods : Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Results : Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms w as found in the range of 0.001-1.0 ${\mu}g$/mL. The limit of detection (S/N=3) was 0.001 ${\mu}g$/mL and limit of quantification was 0.01 ${\mu}g$/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. Conclusion : This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

• Journal of Food Hygiene and Safety
• /
• v.29 no.2
• /
• pp.123-130
• /
• 2014

A simultaneous determination was developed for 9 aminoglycoside antibiotics (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygromycin B, kanamycin, neomycin, spectinomycin, and streptomycin) in meat by liquid chromatography tandem mass spectrometry (LC-MS/MS). Each parameter was established by multiple reaction monitoring in positive ion mode. The developed method was validated for specificity, linearity, accuracy, and precision based on CODEX validation guideline. Linearity was over 0.98 with calibration curves of the mixed standards. Recovery of 9 aminoglycosides ranged on 60.5~114% for beef, 60.1~112% for pork and 63.8~131% for chicken. The limit of detection (LOD) and limit of quantification (LOQ) were 0.001~0.009 mg/kg and 0.006~0.03 mg/kg, respectively in livestock products including beef, pork and chicken. This study also performed survey of residual aminoglycoside antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Aminoglycosides were not found in any of the samples.

• Journal of Food Hygiene and Safety
• /
• v.34 no.2
• /
• pp.140-147
• /
• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• Journal of Food Hygiene and Safety
• /
• v.34 no.3
• /
• pp.227-234
• /
• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

• Korean Journal of Soil Science and Fertilizer
• /
• v.21 no.4
• /
• pp.386-408
• /
• 1988

A study was conducted to develop a model for estimating evapotranspiration and yield of Chinese cabbages from meteorological factors from 1981 to 1986 in Suweon, Korea. Lysimeters with water table maintained at 50cm depth were used to measure the potential evapotranspiration and the maximum evapotranspiration in situ. The actual evapotranspiration and the yield were measured in the field plots irrigated with different soil moisture regimes of -0.2, -0.5, and -1.0 bars, respectively. The soil water content throughout the profile was monitored by a neutron moisture depth gauge and the soil water potentials were measured using gypsum block and tensiometer. The fresh weight of Chinese cabbages at harvest was measured as yield. The data collected in situ were analyzed to obtain parameters related to modeling. The results were summarized as followings: 1. The 5-year mean of potential evapotranspiration (PET) gradually increased from 2.38 mm/day in early April to 3.98 mm/day in mid-June, and thereafter, decreased to 1.06 mm/day in mid-November. The estimated PET by Penman, Radiation or Blanney-Criddle methods were overestimated in comparison with the measured PET, while those by Pan-evaporation method were underestimated. The correlation between the estimated and the measured PET, however, showed high significance except for July and August by Blanney-Criddle method, which implied that the coefficients should be adjusted to the Korean conditions. 2. The meteorological factors which showed hgih correlation with the measured PET were temperature, vapour pressure deficit, sunshine hours, solar radiation and pan-evaporation. Several multiple regression equations using meteorological factors were formulated to estimate PET. The equation with pan-evaporation (Eo) was the simplest but highly accurate. PET = 0.712 + 0.705Eo 3. The crop coefficient of Chinese cabbages (Kc), the ratio of the maximum evapotranspiration (ETm) to PET, ranged from 0.5 to 0.7 at early growth stage and from 0.9 to 1.2 at mid and late growth stages. The regression equation with respect to the growth progress degree (G), ranging from 0.0 at transplanting day to 1.0 at the harvesting day, were: $$Kc=0.598+0.959G-0.501G^2$$ for spring cabbages $$Kc=0.402+1.887G-1.432G^2$$ for autumn cabbages 4. The soil factor (Kf), the ratio of the actual evapotranspiration to the maximum evapotranspiration, showed 1.0 when the available soil water fraction (f) was higher than a threshold value (fp) and decreased linearly with decreasing f below fp. The relationships were: Kf=1.0 for $$f{\geq}fp$$ Kf=a+bf for f$$I{\leq}Esm$$ Es = Esm for I > Esm 6. The model for estimating actual evapotranspiration (ETa) was based on the water balance neglecting capillary rise as: ETa=PET. Kc. Kf+Es 7. The model for estimating relative yield (Y/Ym) was selected among the regression equations with the measured ETa as: Y/Ym=a+bln(ETa) The coefficients and b were 0.07 and 0.73 for spring Chinese cabbages and 0.37 and 0.66 for autumn Chinese cabbages, respectively. 8. The estimated ETa and Y/Ym were compared with the measured values to verify the model established above. The estimated ETa showed disparities within 0.29mm/day for spring Chinese cabbages and 0.19mm/day for autumn Chinese cabbages. The average deviation of the estimated relative yield were 0.14 and 0.09, respectively. 9. The deviations between the estimated values by the model and the actual values obtained from three cropping field experiments after the completion of the model calibration were within reasonable confidence range. Therefore, this model was validated to be used in practical purpose.