• Analytical Science and Technology
• /
• v.29 no.4
• /
• pp.179-185
• /
• 2016

An effective analytical method has been developed for the determination of β-blockers(atenolol, metoprolol and propranolol) and 6 β-lactams(amoxicillin, penicillin G, cefaclor, cefadroxil, cephalexin and cephradine) in water samples using two different cartridges. The samples were extracted by solid-phase extraction (SPE) with the usage of polymeric hydrophile-lipophile balance(HLB cartridges) and strong cation-exchange mixed-mode polymeric sorbent (MCX cartridges). A XDB-C₁₈ column(1.8 μm; 3.0 mm × 100 mm) was used for the sufficient chromatographic resolution. The calibration curves showed good linearity with high correlation coefficients (>0.995). The method detection limits (MDL) and the limits of quantification(LOQ) were from 1.1 to 3.9 ng/L and from 5 to 13 ng/L, respectively. The method was applied for the determination of the target compounds in tributaries and raw water of the Han River and these were found at N.D. to 0.209 μg/L.

• Analytical Science and Technology
• /
• v.24 no.1
• /
• pp.10-14
• /
• 2011

This study was performed to compare international analytical methods of bromide and applied to determine bromide in bottled mineral water and raw ground water in Korea. Bromide in water was eluted by 10~50 mM potassium hydroxide (KOH) and determined by ion chromatography-suppressed conductivity detector (IC-CD). Sample was purified with Ba- and H-on-guard cartridge and $0.2\;{\mu}m$ membrane filter. The method detection limit (MDL) and the limit of quantitation (LOQ) of bromide were 0.2 and $0.5\;{\mu}g/L$, respectively. The calibration curve showed good lineality above 0.9993 in the ranges of the $0.5\sim80\;{\mu}g/L$. A correlation coefficient of bromide in ground water and sum of bromide and bromate in bottled mineral water is 0.808.

• Journal of Food Hygiene and Safety
• /
• v.36 no.5
• /
• pp.376-381
• /
• 2021

Red beet (Beta vulgaris L.) is a root vegetable and a popular functional food ingredient of dark red-purple appearance due largely to betacyanins, principally betanine (75-95%) and its isomer, isobetanine (15-45%). This study developed an analytical method for beet red in terms of betanine and isobetanine in processed food products labeled with beet red as a food additive. High Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) was used with a C₁₈ column. Linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision and uncertainty in measurement were calculated for method validation. Matrix-matched calibration was applied to the candy, ice cream, and cocoa product, respectively, and R² was ≥0.9998, showing a high level of linearity. The LOD and LOQ were 0.16 to 0.32 and 0.48 to 0.97 mg/L, respectively. As a result of repeated intra-day and interday experiments to validate the accuracy and precision of the analytical method, the recovery rates were 96.0-103.1% and 100.0-102.2%, respectively and the RSD% was 0.5-3.3% and 0.9-3.8%, respectively. Moreover, the measurement uncertainty was estimated to be 1.71-12.43% depending on the matrix and the measured concentration. In this study, betanine and isobetanine were quantified (8.4-3,823.4 mg/kg) by applying the developed analytical method to processed food products (n= 26; e.g., candy, ice cream, and other processed foods) labeled with beet red as a food additive.

• Journal of Food Hygiene and Safety
• /
• v.34 no.4
• /
• pp.334-339
• /
• 2019

A procedure based on high-performance liquid chromatography (HPLC) is described to determine ${\beta}-carotene$ in infant formulas. The method for ${\beta}-carotene$ analysis was performed on a C18 reversed-phase column using acetonitrile/methanol/dichloromethane (6:1:3, v/v/v) as a mobile phase. ${\beta}-Carotene$ was determined in HPLC with photo diode array (PDA) detector. The parameters of validation were specificity, linearity, LOD, LOQ, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity ($R^2$), which was over 0.999 in the range of 0.125~2 mg/L. The detection and quantification limits were 0.064 and 0.193 mg/L, respectively. The accuracy and precision of this method using an STD spiked sample were 80~119% and 1.02~2.05% respectively. The method was applied to the analysis of various infant formula and follow-up formulas products containing ${\beta}-carotene$, and all the products contained acceptable levels of ${\beta}-carotene$ for nutrition labeling.

• Analytical Science and Technology
• /
• v.32 no.2
• /
• pp.35-47
• /
• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• Journal of the Korean Society of International Agriculture
• /
• v.30 no.4
• /
• pp.339-346
• /
• 2018

Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

• Korean Journal of Plant Resources
• /
• v.34 no.4
• /
• pp.384-394
• /
• 2021

The aim of this study was to investigate the correlation between soil properties and marker compounds contents of Paeonia lactiflora. The methods of determining marker compounds were validated by measuring the linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and recovery using UPLC analysis. P. lactiflora contained albiflorin at 0.04 ± 0.00 ~ 2.79 ± 0.21%, paeoniflorin at 1.98 ± 0.14 ~ 6.67 ± 0.84%. The root dry weight (RDW) of P. lactiflora was 0.06 ± 0.02 ~ 1.27 ± 0.28 kg. The soil properties analysis such as soil pH, electric conductivity (EC), organic matter (OM), total nitrogen (TN), available phosphate (Avail. P₂O₅), exchangeable cation and cation exchange capacity (CEC) were performed following standard analysis manual. The results of correlation analysis between soil properties and growth characteristics, available P₂O₅ was positively coreelated with the RDW of P. lactiflora. On the other hand, the RDW of P. lactiflora showed significantly negative correlation with contents of albiflorin and paeoniflorin. The results of this study was might be help to provide useful information on the establish of standard cultivation by the investigate correlation analysis between growth characteristics and marker compound contents of P. lactiflora.

• Journal of Food Hygiene and Safety
• /
• v.36 no.6
• /
• pp.474-480
• /
• 2021

Sodium alginate is the sodium salt of alginic acid, commonly used as a food additive for stabilizing, thickening, and emulsifying properties. A relatively simple and universal analysis method is used to study sodium alginate due to the complex pretreatment process and extended analysis time required during the quantitative method. As for the equipment, HPLC-UVD and Unison US-Phenyl column were used for analysis. For the pretreatment condition, a shaking apparatus was used for extraction at 150 rpm for 180 minutes at room temperature. The calibration curve made from the standard sodium alginate solution in 5 concentration ranges showed that the linearity (R²) is 0.9999 on average. LOD and LOQ showed 3.96 mg/kg and 12.0 mg/kg, respectively. Furthermore, the average intraday and inter-day accuracy (%) and precision (RSD%) were 98.47-103.74% and 1.69-3.08% for seaweed jelly noodle samples and 99.95-105.76% and 0.59-3.63% for sherbet samples, respectively. The relative uncertainty value was appropriate for the CODEX standard with 1.5-7.9%. To evaluate the applicability of the method developed in this study, the sodium alginate concentrations of 103 products were quantified. The result showed that the detection rate is highest from starch vermicelli and instant fried noodles to sugar processed products.

• Korean Journal of Pharmacognosy
• /
• v.53 no.3
• /
• pp.162-169
• /
• 2022

This study investigated the mycotoxins (aflatoxin B₁, B₂, G₁, G₂, fumonisin B₁, B₂, ochratoxin A and zearalenone) contained in edible and medicinal plants in Seoul Yangnyeong market during 2020-2021. We analyzed contamination of mycotoxins using LC-MS/MS and evaluated risk assessment. The method was validated by assessing matrix effects, linearity, limit of detection (LOD), limit of quantification(LOQ) and recovery. Matrix-matched standard calibration was used for calibration curves showed good linearity (r²>0.999). The LOD, LOQ and recovery were 0.01-0.23 ㎍/kg, 0.04-0.71 ㎍/kg and 75.5-117.9% respectively. Mycotoxins were detected in 22 of 171 samples; aflatoxin B₁ (6.66 ㎍/kg), fumonisin (7.54-64.68 ㎍/kg), ochratoxin A (4.21-10.56 ㎍/kg) and zearalenone (7.31-60.76 ㎍/kg). In the risk assessment, the MOE (Margine of Exposure) of aflatoxin B₁ and ochratoxin A were in the range of 1.48×10³-2.36×10⁵. No items exceeded 100% in %TDI (Tolerable Daily Intake) of fumonisin (B₁+B₂) and zearalenone.

• Journal of the Society of Cosmetic Scientists of Korea
• /
• v.48 no.4
• /
• pp.321-330
• /
• 2022

This study attempted to establish an optimal multi-compound simultaneous analysis method that can secure reliable results for 15 - preservatives, 2 - sun screens and 1 - antioxidants of cosmetics using HPLC-PDA. Since the potential of hydrogen (pH) in the mobile phase affects the acid dissociation constant (pKa) of the preservatives, and the peak retention time shift and area change were observed. The peak separation condition was established by adjusting the pH to 0.1% H₃PO₄ addition (mL) when preparing the mobile phase. As a results of method validation, the linearity correlation coefficient (R²) of above 0.999 were obtained, and accuracy 87.9 ~ 101.1%, 0.1 ~ 7.6% precision for two types of cosmetics (cream and shampoo). It was found that the limit of detection (LOD) was 0.1 ~ 0.2 mg/kg and the limit of quantitation (LOQ) was 2.0 ~ 4.0 mg/kg. In addition, it was possible to simultaneously separate p-anisic acid, a natural compound that was difficult to separate in HPLC due to the small difference from methylparaben, a synthetic preservatives. Through this study, it will be effectively used to secure quality control and safety for compound that need restrictions on use cosmetics.