• Journal of Food Hygiene and Safety
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• v.27 no.1
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• pp.37-41
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• 2012

The current standard for testing tetrodotoxin (TTX) in foodstuffs is the mouse bioassay (MBA) in Korea as in many other countries. However, this test suffers from potential ethical concerns over the use of live animals. In addition, the mouse bioassay does not test for a specific toxin thus a sample resulting in mouse incapacitation would need further confirmatory testing to determine the exact source toxin (e.g., TTX, STX, brevotoxin, etc.). Furthermore, though the time of death is proportional to toxicity in this assay, the dynamic range for this proportional relationship is small thus many samples must be diluted and new mice be injected to yield a result that falls within the quantitative dynamic range. Therefore, in recent years, there have been many efforts in this field to develop alternative assays. High performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) has been emerged as one of the most promising options. A LC-MS-MS method involves solid-phase extraction (SPE) and followed by analysis using an electrospray in the positive ionization mode and multiple reactions monitoring (MRM). To adopt LC-MS-MS method as alternative standard for testing TTX, we performed a validation study for the quantification of TTX in puffer fish. This LC-MS-MS method showed good sensitivity as limits of detection (LOD) of $0.03{\sim}0.08{\mu}g/g$ and limits of quantification (LOQ) of $0.10{\sim}0.25{\mu}g/g$. The linearity ($r^2$) of tetrodotoxin were 0.9986~0.9997, the recovery were 80.9~103.0% and the relative standard deviations (RSD) were 4.3~13.0%. The correlation coefficient between the mouse bioassay and LC/MS/MS method was higher than 0.95.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.418-423
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• 2017

An analytical method for the determination of dexamethasone (DM) in bovine milk samples was developed and validated using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Milk samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase $C_{18}$ column with gradient elution using a mobile phase of 0.1% formic acid in 95% acetonitrile. The procedure was validated according to the Ministry of Food and Drug Safety guideline determining accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). Mean recoveries of DM from spiked milk samples (25, 125, and 1,250 ng/mL) were 98.9-109.6%, and the relative standard deviation was between 1.7 and 4.4%. Linearity in concentration range of 12.5-1,250 ng/mL was obtained with the correlation coefficient ($r^2$) of 0.9997. LOD and LOQ for the investigated DM were 0.15 and 0.5 ng/mL depending on milk samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of DM residues in bovine milk.

• Analytical Science and Technology
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• v.23 no.2
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• pp.155-160
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• 2010

This study was performed to compare international analytical methods of bromate and applied to determine bromate in bottled mineral water in Korea. Bromate in bottled mineral water was eluted by 10~50 mM potassium hydroxide (KOH) and determined by ion chromatograph-suppressed conductivity detector (ICCD). Sample was purified with on guard Ba-, Ag- and H-cartridges and $0.2\;{\mu}m$ membrane filter. The method detection limit (MDL) and the limit of quantitation (LOQ) of bromate were 0.1 and $0.5\;{\mu}g/L$, respectively. The calibration curve showed good lineality above 0.9998 in the ranges of the $0.5\sim40\;{\mu}g/L$. Bromate from 33 samples among total 157 bottled mineral water samples was detected in the concentration range of $0.5\sim6.5\;{\mu}g/L$. The detected concentrations were within bottled mineral water quality criteria ($10\;{\mu}g/L$) in Korea.

• Analytical Science and Technology
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• v.30 no.5
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• pp.295-302
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• 2017

This study presents a method validation for extraction and quantitative analysis of levulinic acid in soy sacues using high performance liquid chromatograph-photodiode array detector (HPLC-PDA). The levulinic acid in samples were extracted with distilled water, and then purified with C18 Sep-Pak cartridge. The calibration curves showed good linearity (R > 0.999) in a relatively wide concentration range ($2.5-400{\mu}g/mL$). Mean recoveries and relative standard deviation (RSD) of levulinic acid spiked in soy sauce samples at different spiking levels ($2.5-400{\mu}g/mL$; 6 point). Recoveries were 87.58-97.26 % with RSD less than 15 %, and limit of detection (LOD) and limit of quantification (LOQ) were 0.64 and $1.64{\mu}g/mL$, respectively. According to monitoring result with the established method, levulinic acid was found in 43 of 59 domestic commercial soy sauces, soy sauce based sauces and seasoned meats. The contamination levels were 0.44-1.23 mg/mL for soy sauces, 0.03-0.83 mg/mL for soy sauce based sauces and 8.43-38.94 mg/mL for seasoned meats. The results indicated to be rapidly and accurately qualifying levulinic acid and can be used as a suitable quality control method for soy sauce and soy sauce related commodities.

• Journal of Food Hygiene and Safety
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• v.35 no.4
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• pp.398-410
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• 2020

In this study, the contents of soluble vitamins B₁ (thiamin), B₂ (riboflavin), and B₃ (niacin) in 13 kinds of rice, 11 kinds of noodles, and 15 kinds of sauces were identified. The limit of detection (LOD) and limit of quantification (LOQ) were checked to determine the reliability of the experimental results, and the accuracy of the results through the standard reference material (SRM 1849a) was verified to show excellent indicators. As for thiamin, japchaebab (stir-fried glass noodles with rice) was found to contain the highest content among rice dishes, makguksu (buckwheat noodles) among noodle dishes, and tomato spaghetti sauce among sauces. Riboflavin was identified as having the highest content in slightly spicy jajangbab (black-bean sauce with rice), bibimguksu (spicy noodles) for noodles, and spicy curry with turmeric for sauces. Niacin was highest in content in the deep and rich flavors of spicy chicken-fried rice, janchiguksu (banquet noodles), and black-bean sauce, respectively. As a result of checking the amount of recommended daily intake of water-soluble vitamins for Korean adult men and women, the highest content of riboflavin was 217.40% for men and 271.75% for women. Through this study, we are going to establish a database of nutrients for the water-soluble vitamins contained in rice, noodles, and sauces to provide the necessary dietary data concerning the content of the water-soluble vitamins contained in foods for daily recommended intake.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.502-506
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• 2011

Most countries have the legislation and regulation for POPs control in food. In here, we studied the quantitative analysis of 24 organochlorine POPs (${\alpha}$-HCH 1, ${\beta}$-HCH 2, ${\gamma}$-HCH 3, ${\delta}$-HCH 4, trans-chlrodane 5, 2,4'-DDE 6, ${\alpha}$-endosulfan 7, cis-chlordane 8, 2,4'-DDD 9, endrin 10, ${\beta}$-endosulfan 11, 2,4'-DDT 12, endosulfan sulfate 13, HCB 14, aldrin 15, trans-nonachlor 16, 4,4'-DDE 17, dieldrin 18, 4,4'-DDD 19, cis-nonachlor 20, 4,4'-DDT 21, heptachlor 22, heptachlor epoxide 23 and mirex 24) with GC-ECD. The retention time of analytes were ranged between 19.18 min and 34.69 min, and their peak intervals were over 0.05 min at least. LOQs were ranged 0.003 ~ 0.033 ng/g, and their recovery rates were showed 60.9 ~ 120.8% on the 0.1 ng/g concentration of 24 organochlorine POPs. All tested 30 sundried salts were collected on Korean retailed market, and any analyte was not found in all the samples on LOQ levels.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.148-155
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• 2014

The transfer pattern of chlorpyrifos present in soil to cucumber plants were assessed and reported with plant growth, concentration dependency, and duration. Cucumber seedlings cultivated in a growth chamber for 30 days and a greenhouse for 120 days. Weight and length of cucumbers cultivated in the chamber increased with the increasing time, while the uptake of chlorpyrifos by cucumber increased a period from 0 to 15 days and decreased after 15 days. Uptake rates of chlorpyrifos into a cucumber plant were 1.0~1.3% to initial amounts treated with 20 and 40 mg/kg to soil. Most chlorpyrifos residues were detected in root, followed by stem and leaf. Results of the greenhouse test showed that chlorpyrifos amounts in cucumber fruits were present less than LOQ (0.02 mg/kg), and chlorpyrifos was mainly found in the root of the cucumber plant. Chlorpyrifos absorbed in a cucumber under greenhouse condition was smaller than that in chamber condition as 0.03~0.04%. Degradation patterns of chlorpyrifos in soils were similar during indoor and outdoor tests with half-lives of 25.8~73.0 days. These results may be useful for establishing the management strategy of residual pesticides in soil environment.

• YAKHAK HOEJI
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• v.52 no.6
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• pp.419-425
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• 2008

A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

• Journal of the Korean Chemical Society
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• v.57 no.1
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• pp.40-51
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• 2013

In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were $2.58{\mu}g/L$ and $7.82{\mu}g/L$, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the $r^2$ value was 0.9992 in the concentration range of $7.82-100{\mu}g/L$, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the $^{19}F$ NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.

• Korean Journal of Environmental Agriculture
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• v.30 no.4
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• pp.446-452
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• 2011

BACKGROUND: To investigate the dissipation patterns of 3 pesticides, azoxystrobin, difenoconazole and iprodione, on green garlic after field treatment pesticides were treated as foliar treatment by single application at recommended and double the recommended rates. METHODS AND RESULTS: Residue samples were harvested at 0, 1, 2, 5, 7 and 10 days post-treatment for azoxystrobin and 0, 1, 2, 5, 7, 10, 15 and 21 days post-treatment for difenoconazole and iprodione. After preparation the fortified samples were extracted and analyzed by gas chromotography-electron capture detector (GC-ECD) to determine the residue levels. Recoveries ranged from 87 to 109% for azoxystrobin, difenoconazole and iprodione at two different levels. The limit of Quantification (LOQ) values were 0.002 mg/kg for azoxystrobin and difenoconazole and 0.01 mg/kg for iprodione. CONCLUSION(S): Half-lives of azoxystrobin, difenoconazole and iprodione in green garlic after treatment were 1.2, 3.8 and 3.2 days at recommended and 1.4, 3.3 and 3.2 at double the recommended rate, respectively. Residue level of azoxystrobin, difenoconazole and iprodione in green garlic were below the maximum residue limits (MRLs) at 0 day, 0 day and 5 days, respectively. Therefore, these pesticide were considered that residues was satisfied to the requirement of domestic trade related to the consumer safety.