• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.124-130
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• 2018

The Ministry of Food and Drug Safety (MFDS) is amending its test methods for the use of health functional foods (dietary food supplement), in order to establish regulatory standards and specifications in Korea. In this regard, we continue to pursue and perform our research on the analytical method development for the items being researched and reviewed. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determinate six major bioactive flavonolignans in silymarin, which are based on the use of a liquid chromatographic-tandem mass spectrometry (LC-MS/MS). The standard calibration curves presented a linearity effect with the correlation coefficient ($r^2$) > 0.999. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $0.3{\sim}9.0{\mu}g/L$ and $0.8{\sim}27.3{\mu}g/L$, respectively. The recovery results ranged between 96.2~98.6% at 3 different concentration levels, and its relative standard deviations (RSDs) were less than 5% as noted in this study. The proposed analytical method was characterized with a noted high resolution of the individual silymarin constituents, and the assay was fully validated as well. Our research can provide a significant scientific evidence that can be useful to amend the silymarin test method for the Health Functional Food Code.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.22-29
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• 2019

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

• The Korean Journal of Nuclear Medicine Technology
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• v.25 no.2
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• pp.15-24
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• 2021

Purpose SPECT/CT was noted for its excellent correction method and qualitative functions based on fusion images in the early stages of dissemination, and interest in and utilization of quantitative functions has been increasing with the recent introduction of companion diagnostic therapy(Theranostics). Unlike PET/CT, various conditions like the type of collimator and detector rotation are a challenging factor for image acquisition and reconstruction methods at absolute quantification of SPECT/CT. Therefore, in this study, We want to find out the effect on the radioactivity concentration estimate by the increase or decrease of the total acquisition time according to the number of projections and the acquisition time per projection among SPECT/CT imaging conditions. Materials and Methods After filling the 9,293 ml cylindrical phantom with sterile water and diluting 99mTc 91.76 MBq, the standard image was taken with a total acquisition time of 600 sec (10 sec/frame × 120 frames, matrix size 128 × 128) and also volume sensitivity and the calibration factor was verified. Based on the standard image, the comparative images were obtained by increasing or decreasing the total acquisition time. namely 60 (-90%), 150 (-75%), 300 (-50%), 450 (-25%), 900 (+50%), and 1200 (+100%) sec. For each image detail, the acquisition time(sec/frame) per projection was set to 1.0, 2.5, 5.0, 7.5, 15.0 and 20.0 sec (fixed number of projections: 120 frame) and the number of projection images was set to 12, 30, 60, 90, 180 and 240 frames(fixed time per projection:10 sec). Based on the coefficients measured through the volume of interest in each acquired image, the percentage of variation about the contrast to noise ratio (CNR) was determined as a qualitative assessment, and the quantitative assessment was conducted through the percentage of variation of the radioactivity concentration estimate. At this time, the relationship between the radioactivity concentration estimate (cps/ml) and the actual radioactivity concentration (Bq/ml) was compared and analyzed using the recovery coefficient (RC_Recovery Coefficients) as an indicator. Results The results [CNR, radioactivity Concentration, RC] by the change in the number of projections for each increase or decrease rate (-90%, -75%, -50%, -25%, +50%, +100%) of total acquisition time are as follows. [-89.5%, +3.90%, 1.04] at -90%, [-77.9%, +2.71%, 1.03] at -75%, [-55.6%, +1.85%, 1.02] at -50%, [-33.6%, +1.37%, 1.01] at -25%, [-33.7%, +0.71%, 1.01] at +50%, [+93.2%, +0.32%, 1.00] at +100%. and also The results [CNR, radioactivity Concentration, RC] by the acquisition time change for each increase or decrease rate (-90%, -75%, -50%, -25%, +50%, +100%) of total acquisition time are as follows. [-89.3%, -3.55%, 0.96] at - 90%, [-73.4%, -0.17%, 1.00] at -75%, [-49.6%, -0.34%, 1.00] at -50%, [-24.9%, 0.03%, 1.00] at -25%, [+49.3%, -0.04%, 1.00] at +50%, [+99.0%, +0.11%, 1.00] at +100%. Conclusion In SPECT/CT, the total coefficient obtained according to the increase or decrease of the total acquisition time and the resulting image quality (CNR) showed a pattern that changed proportionally. On the other hand, quantitative evaluations through absolute quantification showed a change of less than 5% (-3.55 to +3.90%) under all experimental conditions, maintaining quantitative accuracy (RC 0.96 to 1.04). Considering the reduction of the total acquisition time rather than the increasing of the image acquiring time, The reduction in total acquisition time is applicable to quantitative analysis without significant loss and is judged to be clinically effective. This study shows that when increasing or decreasing of total acquisition time, changes in acquisition time per projection have fewer fluctuations that occur in qualitative and quantitative condition changes than the change in the number of projections under the same scanning time conditions.

• Journal of Food Hygiene and Safety
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• v.37 no.2
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• pp.39-45
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• 2022

This study aimed to investigate the validation and modify the analytical method to determine quercetin-3-𝑜-gentiobioside and isoquercitrin in Abelmoschus esculentus L. Moench for the standardization of ingredients in development of functional health products. The analytical method was validated based on the ICH (International Conference for Harmonization) guidelines to verify the reliability and validity there of on the specificity, linearity, accuracy, precision, detection limit and quantification limit. For the HPLC analysis method, the peak retention time of the index component of the standard solution and the peak retention time of the index component of A. esculentus L. Moench powder sample were consistent with the spectra thereof, confirming the specificity. The calibration curves of quercetin-3-𝑜-gentiobioside and isoquercitrin showed a linearity with a near-one correlation coefficient (0.9999 and 0.9999), indicating the high suitability thereof for the analysis. A. esculentus L. Moench powder sample of a known concentration were prepared with low, medium, and high concentrations of standard substances and were calculated for the precision and accuracy. The precision of quercetin-3-𝑜-gentiobioside and isoquercitrin was confirmed for intra-day and daily. As a result, the intra-day precision was found to be 0.50-1.48% and 0.77-2.87%, and the daily precision to be 0.07-3.37% and 0.58-1.37%, implying an excellent precision at level below 5%. As a result of accuracy measurement, the intra-day accuracy of quercetin-3-𝑜-gentiobioside and isoquercitrin was found to be 104.87-109.64% and the daily accuracy thereof was found to be 106.85-109.06%, reflecting high level of accuracy. The detection limits of quercetin-3-𝑜-gentiobioside and isoquercitrin were 0.24 ㎍/mL and 0.16 ㎍/mL, respectively, whereas the quantitation limits were 0.71 ㎍/mL and 0.49 ㎍/mL, confirming that detection was valid at the low concentrations as well. From the analysis, the established analytical method was proven to be excellent with high level of results from the verification on the specificity, linearity, precision, accuracy, detection limit and quantitation limit thereof. In addition, as a result of analyzing the content of A. esculentus L. Moench powder samples using a validated analytical method, quercetin-3-𝑜-gentiobioside was analyzed to contain 1.49±0.01 mg/dry weight g, while isoquercitrin contained 1.39±0.01 mg/dry weight g. The study was conducted to verify that the simultaneous analysis on quercetin-3-𝑜-gentiobioside and isoquercitrin, the indicators of A. esculentus L. Moench, is a scientifically reliable and suitable analytical method.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.314-334
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• 2013

This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

• Journal of The Korean Society of Grassland and Forage Science
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• v.36 no.4
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• pp.333-339
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• 2016

The objective of this study was to optimize analytical methods for ochratoxin A (OTA) and zearalenone (ZEA) in rice straw silage and winter forage crops using ultra-high performance liquid chromatography (UHPLC). Samples free of mycotoxins were spiked with $50{\mu}g/kg$, $250{\mu}g/kg$, or $500{\mu}g/kg$ of OTA and $300{\mu}g/kg$, $1500{\mu}g/kg$, or $3000{\mu}g/kg$ of ZEA. OTA and ZEA were extracted by acetonitrile and cleaned-up using an immunoaffinity column. They were then subjected to analysis with UHPLC equipped with a fluorescence detector. The correlation coefficients of calibration curves showed high linearity ($R^2{\geq_-}0.9999$ for OTA and $R^2{\geq_-}0.9995$ for ZEA). The limit of detection and quantification were $0.1{\mu}g/kg$ and $0.3{\mu}g/kg$, respectively, for OTA and $5{\mu}g/kg$ and $16.7{\mu}g/kg$, respectively, for ZEA. The recovery and relative standard deviation (RSD) of OTA were as follows: rice straw = 84.23~95.33%, 2.59~4.77%; Italian ryegrass = 79.02~95%, 0.86~5.83%; barley = 74.93~97%, 0.85~9.19%; rye = 77.99~96.67%, 0.33~6.26%. The recovery and RSD of ZEA were: rice straw = 109.6~114.22%, 0.67~7.15%; Italian ryegrass = 98.01~109.44%, 1.65~4.81%; barley = 98~113.53%, 0.25~5.85%; rye = 90.44~108.56%, 2.5~4.66%. They both satisfied the standards of European Commission criteria (EC 401-2006) for quantitative analysis. These results showed that the optimized methods could be used for mycotoxin analysis of forages.

• Journal of Food Hygiene and Safety
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• v.33 no.4
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• pp.266-271
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• 2018

The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Analytical Science and Technology
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• v.28 no.6
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• pp.436-445
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• 2015

Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.

• The Journal of the Korea Contents Association
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• v.9 no.12
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• pp.742-749
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• 2009

The use of cone-beam computed tomography(CBCT) has been proposed for guiding the delivery of radiation therapy. A kilovoltage imaging system capable of radiography, fluoroscopy, and cone-beam computed tomography(CT) has been integrated with a medical linear accelerator. A standard clinical linear accelerator, operating in arc therapy mode, and an amorphous-silicon (a-Si) with an on-board electronic portal imager can be used to treat palliative patient and verify the patient's position prior to treatment. On-board CBCT images are used to generate patient geometric models to assist patient setup. The image data can also, potentially, be used for dose reconstruction in combination with the fluence maps from treatment plan. In this study, the accuracy of Hounsfield Units of CBCT images as well as the accuracy of dose calculations based on CBCT images of a phantom and compared the results with those of using CT simulator images. Phantom and patient studies were carried out to evaluate the achievable accuracy in using CBCT and CT stimulator for dose calculation. Relative electron density as a function of HU was obtained for both planning CT stimulator and CBCT using a Catphan-600 (The Phantom Laboratory, USA) calibration phantom. A clinical treatment planning system was employed for CT stimulator and CBCT based dose calculations and subsequent comparisons. The dosimetric consequence as the result of HU variation in CBCT was evaluated by comparing MU/cCy. The differences were about 2.7% (3-4MU/100cGy) in phantom and 2.5% (1-3MU/100cGy) in patients. The difference in HU values in Catphan was small. However, the magnitude of scatter and artifacts in CBCT images are affected by limitation of detector's FOV and patient's involuntary motions. CBCT images included scatters and artifacts due to In addition to guide the patient setup process, CBCT data acquired prior to the treatment be used to recalculate or verify the treatment plan based on the patient anatomy of the treatment area. And the CBCT has potential to become a very useful tool for on-line ART.)