• Title/Summary/Keyword: LOD and LOQ

Search Result 298, Processing Time 0.021 seconds

Analysis of the 6-gingerol Content in Zingiber spp. and their Commercial Foods using HPLC

  • Cho, Sunghun;Lee, Dong Gu;Lee, Sullim;Chae, Sungwook;Lee, Sanghyun
    • Journal of Applied Biological Chemistry
    • /
    • v.58 no.4
    • /
    • pp.377-381
    • /
    • 2015
  • The content analysis of 6-gingerol, which is an active compound, in Zingiber spp. (Z. officinale and Z. mioga) and their commercial foods (ginger teas and powders) was conducted using high-performance liquid chromatography. A reverse phase system was used, with a gradient solvent system of water and acetonitrile. The 6-gingerol content was highest in the methanol extract of Z. officinale root (17.09 mg/g extract) and ginger powder B (15.92 mg/g extract). The results demonstrated that this method was simple and reliable for the quality control of Zingiber commercial foods.

Gas Chromatographic Analysis and Cholinesterase Activity of the Essential Oil from Korean Agastache rugosa (기체크로마토그래피에 의한 한국산 배초향의 정유 분석과 Cholinesterase 억제활성)

  • Choi, Jae Sue;Song, Byong-Min;Park, Hee-Juhn
    • Korean Journal of Pharmacognosy
    • /
    • v.47 no.2
    • /
    • pp.192-196
    • /
    • 2016
  • The herb of Agastache rugosa (Lamiaceae) called Korean mint as a spice or Agastache Herba as a crude drug is known to contain highly fragrant volatile substances. This research aimed to establish the quantitative gas chromatography (GC) method on the essential oil of A. rugosa using the three standard compounds, estragole, methyleugenol, pulegone, and to find whether the essential oil has anti-Alzheimer's activity. The GC quantification method was established by determining the linearity of calibration curve ($R^2$), linear range, and both limit-of-detection (LOD) and limit-of-quantification (LOQ). The $IC_{50}$ of the essential oil on the activities of acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) were determined to be $69.06{\pm}0.26$ and $76.71{\pm}0.58{\mu}g/ml$, respectively.

Development of a Chloroform Reference Material for the Proficiency Testing of Hazardous Compounds in Commercial Consumer Chemical Products Under the Consumer Chemical Products and Biocide Safety Management Act (K-BPR)

  • Lee, Sang Tak;Lee, Jae-ung;Kim, Joo-Hyon;Oh, Han Bin
    • Mass Spectrometry Letters
    • /
    • v.10 no.4
    • /
    • pp.112-116
    • /
    • 2019
  • In this study, a chloroform consumer chemical product (CCP) reference material (RM) is successfully developed, with potential to be used in the proficiency testing of hazardous compounds in CCPs for analysis and testing agencies. Validation experiments are rigorously conducted to evaluate whether the RM meets the requirements set by the ISO 13528 and ISO Guide 35, using a reliable GC/MS method for the analysis of chloroform. The obtained calibration plot linearity, limit of detection (LOD), and limit of quantitation (LOQ) are excellent. The developed RM meets the homogeneity and stability requirements; the between-unit (sbb) and within-unit (swb) standard deviations are less than 2.5%, and the stability is found to be guaranteed for 50 days.

Green flow injection spectrophotometric system for lead ion (II) evaluation in vegetables samples using new azo reagent

  • Fatimah Lateef Al-Zubaidi;Khdeeja Jabbar Ali
    • Analytical Science and Technology
    • /
    • v.36 no.1
    • /
    • pp.1-11
    • /
    • 2023
  • A new, sensitive, and reliable flow injection methodology was investigated for the determination of lead ion (II) in vegetables' samples using a laboratory-prepared reagent 2-[(6-methoxy-2-benzothiazoly)azo]-4-methoxy phenol (6-MBTAMP). Infrared spectroscopy, UV-visible spectrophotometry, Energy dispersive X-ray spectroscopy (EDX), Elemental Analysis (CHN), nuclear magnetic resonance spectroscopy 1HNMR, and 13CNMR techniques were used to characterize the reagent and lead (II) complex. The method is based on lead ion (II) reacting with the reagent (6-MBTAMP) in a neutral solution to produce a green-red complex with a maximum absorbance at 670 nm. The optimum conditions, such as flow rate, lead ion (II) volume, reagent volume, medium pH, reagent concentration, and reaction coil length were thoroughly examined. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.621 mg·L-1 and 2.069 mg·L-1 , respectively, while Sandell's sensitivity was determined to be 0.345 ㎍·cm-2.

Determination of Ursodeoxycholic Acid in Crude Drug Formulations by HPLC and SPE Using Selective Pre-column Derivatization with 2-Bromoacetyl-6-methoxynaphthalene (2-Bromoacetyl-6-methoxynaphthalene을 형광유도체화제로 HPLC와 SPE를 이용한 생약제제 중 Ursodeoxycholic acid의 정량)

  • 진창화;임수희;이기진;심형섭;조의환;염정록
    • YAKHAK HOEJI
    • /
    • v.46 no.6
    • /
    • pp.392-397
    • /
    • 2002
  • A simple and sensitive high performance liquid chromatographic method to quantitate ursodeoxycholic acid in crude drug pharmaceuticals was investigated. Ursodeoxycholic acid react with 2-bromoacetyl-6-methoxynaphthalene (Br-AMN) in the presence of triethylamine to form highly fluorescent derivative. The derivatization procedure was performed at 7$0^{\circ}C$ and completed within 30 min. The optimal wavelength of the fluorescence detector are λ$_{ex}$=300 nm and λ$_{em}$ = 460 nm. The LOD of the ursodeoxycholic acid was 25 ng/mι based on the S/N =3, and the LOQ was 80 ng/mι based on S/N = 10. Crude drug pharmaceuticals pretreated by solid phase extraction (Sep-pak $C_{18}$ cartridge) which were shown very good separation and recovery values for the compound.d.

Melamine testing of meat, eggs and diary products sold in Incheon

  • Ra, Do-Kyung;Hong, Seong-Hee;Lee, Jeong-Gu;Lee, Sung-Mo
    • Korean Journal of Veterinary Service
    • /
    • v.32 no.4
    • /
    • pp.381-383
    • /
    • 2009
  • From Oct. 2008 to Oct. 2009, 619 livestock products sold in Incheon were examined for melamine contamination. HPLC was used to detect the melamine concentration from various products. $C_{18}$ column $(3.9\times150mm,\;4{\mu}m)$ was applied with a phase composed of 10mM citric acid and 10mM sodium octane sulfonate : acetonitrile (in ratio 90:10) pumped isocratically at 1.0ml/min. Melamine was not detected from any of the products at the level of LOD 0.03mg/kg and LOQ 0.08mg/kg, suggesting that no melamine contamination was ascertained in livestock products in Incheon area. However, further tests should be done to detect other melamine analogues for the evaluation of toxicity and safety of melamine and cyanuric acid in the future.

Modification and Validation of an Analytical Method for Dieckol in Ecklonia Stolonifera Extract (곰피추출물의 지표성분 Dieckol의 분석법 개선 및 검증)

  • Han, Xionggao;Choi, Sun-Il;Men, Xiao;Lee, Se-jeong;Oh, Geon;Jin, Heegu;Oh, Hyun-Ji;Kim, Eunjin;Kim, Jongwook;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
    • /
    • v.37 no.3
    • /
    • pp.143-148
    • /
    • 2022
  • This study was to investigate an analytical method for determining dieckol content in Ecklonia stolonifera extract. According to the guidelines of International Conference on Harmonization. Method validation was performed by measuring the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of dieckol using high-performance liquid chromatography-photodiode array. The results showed that the correlation coefficient of calibration curve (R2) for dieckol was 0.9997. The LOD and LOQ for dieckol were 0.18 and 0.56 ㎍/mL, respectively. The intra- and inter-day precision values of dieckol were approximately 1.58-4.39% and 1.37-4.64%, respectively. Moreover, intra- and inter-day accuracies of dieckol were approximately 96.91-102.33% and 98.41-105.71%, respectively. Thus, we successfully validated the analytical method for estimating dieckol content in E. stolonifera extract.

Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

  • Kim, Nam Sook;Yoo, Geum Joo;Kim, Kyu Yeon;Lee, Ji Hyun;Park, Sung-Kwan;Baek, Sun Young;Kang, Hoil
    • 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.

Development and Validation of an Analytical Method for Betanine and Isobetanine in Processed Food Products Labeled with Beet Red

  • Kang, Hyun-Hee;Yun, Choong-In;Lee, Gayeong;Shin, Jae-Wook;Kim, Young-Jun
    • 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.

Determination of Sodium Alginate in Processed Food Products Distributed in Korea

  • Yang, Hyo-Jin;Seo, Eunbin;Yun, Choong-In;Kim, Young-Jun
    • 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.