• Title/Summary/Keyword: limit of detection

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Simultaneous Determination of 8 Preservatives (6 Parabens, 2-Phenoxyethanol, and Chlorphenesin) in Cosmetics by $UPLC^{TM}$ ($UPLC^{TM}$를 이용한 화장품 중 보존제 8종(파라벤 6종, 페녹시에탄올, 클로페네신)의 동시분석)

  • Park, Jeong-Eun;Lee, So-Mi;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.33 no.4
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    • pp.263-267
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    • 2007
  • Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.

Effect of Physical Control Technology on Aspergillus ochraceus Reduction (물리적 제어기술이 Aspergillus ochraceus 저감화에 미치는 영향)

  • Lee, Eun-Seon;Kim, Jong-Hui;Kim, Bu-Min;Oh, Mi-Hwa
    • Journal of Food Hygiene and Safety
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    • v.36 no.5
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    • pp.447-453
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    • 2021
  • In this study, the effectiveness of physical control technology, a combined light sterilization (LED, UV) and hot water treatment in reducing Aspergillus ochraceus for food production environment was investigated. In brief, 1 mL aliquot of A. ochraceus spore suspension (107-8 spore/mL) was inoculated onto stainless steel chips, which was then dried at 37℃, and each was subjected to different physical treatment. Treatments were performed for 0.5, 1, 2, 5, 8, and 11 hours to reduce the strains using a light-emitting diode, but no significant difference was confirmed among the treatments. However, a significant reduction was observed on the chips treated with UV-C exposure and hot water immersion. After being treated solely with 360 kJ/m2 of UV-C on stainless steel chip, the fungi were significantly reduced to 1.27 log CFU/cm2. Concerning the hot water treatment, the initial inoculum amount of 6.49 log CFU/cm2 was entirely killed by immersion in 83℃ water for 5 minutes. Maintaining a high temperature for 5 minutes at the site is difficult. Thus, considering economic feasibility and usability, we attempted to confirm the appropriate A. ochraceus reduction conditions by combining a relatively low temperature of 60℃ and UV rays. With the combined treatments, even in lukewarm water, A. ochraceus decreased significantly through the increases in the immersion time and the amount of UV-C irradiation, and the yield was below the detection limit. Based on these results, if work tools are immersed in 60℃ lukewarm water for 3 minutes and then placed in a UV sterilization device for more than 10 minutes, the possibility of A. ochraceus cross-contamination during work is expected to be reduced.

A study on the calibration characteristics of organic fatty acids designated as new offensive odorants by cryogenic trapping-thermal desorption technique (유기지방산 신규악취물질에 대한 저온농축 열탈착방식 (Thermal desorber)의 검량특성 연구)

  • Ahn, Ji-Won;Kim, Ki-Hyun;Im, Moon-Soon;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.488-497
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    • 2009
  • In this study, analytical methodology for several organic fatty acids (OFA: propionic acid (PA), butyric acid (BA), isovaleric acid (IA), and valeric acid (VA)) designated as new offensive odorants in Korea (as of year 2010) was investigated along with some odorous VOCs (styrene, toluene, xylene, methyl ethyl ketone, methyl isobutyl ketone, butyl acetate, and isobutyl alcohol). For this purpose, working standards (WS) containing all of these 13 compounds were loaded into adsorption tube filled with Tenax TA, and analyzed by gas chromatography (GC) system thermal desorber interfaced with. The analytical sensitivities of organic fatty acids expressed in terms of detection limit (both in absolute mass (ng) and concentration (ppb)) were lower by 1.5-2 times than other compounds (PA: 0.24 ng (0.16 ppb), BA: 0.19 ng (0.11 ppb), IA: 0.15 ng (0.07 ppb), and VA: 0.28 ng (0.13 ppb)). The precision of BA, IA, and VA, if assessed in terms of relative standard error (RSE), maintained above 5%, while the precison of other compounds were below 5%. The reproducibility of analysis improved with the aid of internal standard calibration (PA: $1.1{\pm}0.4%$, BA: $10{\pm}0.46$, IA; $12{\pm}0.3%$, VA: $4{\pm}0.1%$), respectively. The results of this study showed that organic fatty acid can be analyzed using adsorption tube and thermal desorber in a more reliable way to replace alkali absorption method introduced in the odor prevention law of the Korea Ministry of Environment (KMOE).

Quantitative determination of inosine 5'-monophosphate dehydrogenase activity in human peripheral blood mononuclear cells by ion-pair reversed-phase high-performance liquid chromatography (이온쌍 역상 HPLC를 이용한 인체 말초혈액단핵구에서 이노신 5'-일인산 탈수소효소 활성의 정량적 측정)

  • Shin, Hye-Jin;Kwon, Soon-Ho;Park, Ji-Myeong;Kwon, Soon-Hyo;Lee, Kyoung-Ryul;Kim, Young-Jin;Lee, Sang-Hoo
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.531-536
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    • 2010
  • A quantitative analytical method has been established for the measurement of inosine 5'-monophosphate dehydrogenase (IMPDH) activity in human peripheral blood mononuclear cells (PBMCs) by ion-pair reversed-phase high performance liquid chromatography equipped with ultraviolet detection (HPLC/UV). IMPDH is a ${\beta}$-nicotinamide adenine dinucleotide hydrate (NAD+)-dependent dehydrogenase in which the enzyme converts inosine 5'-monophosphate (IMP) into xanthosine 5'-monophosphate (XMP). Its activity was measured by quantifying a HPLC chromatogram corresponding to XMP produced during the incubation of lysed PBMCs with IMP as a substrate and $NAD^+$ as a coenzyme. XMP produced was detected at a wavelength of 260 nm. The mobile phase was composed of a mixture of 37 mM potassium dihydrogen phosphate containing 7 mM tetra-n-butylammonium hydrogen sulfate adjusted to pH 5.5 and methanol (85:15, v/v) with a flow rate of 1 mL/min. The calibration curve was linear ($r^2$=0.999999) in the range of $0.2-50.0\;{\mu}M$ and the limit of quantification (LOQ) was $0.2\;{\mu}M$. The intra- and inter-day precisions were between 0.88-1.47% and 0.85-5.24%, respectively. The intra- and inter-day accuracies were between 98.74-99.99% and 99.95-101.65%, respectively. IMPDH activity in 11 Korean healthy volunteers ranged from 18.29 to 36.60 nmol/h/mg protein (mean = $27.70{\pm}6.28\;nmol/h/mg$ protein).

Improvements in the Environmental Impact Assessment on Seawater and Sediment Qualities for Coastal Dredging Projects (연안준설 사업에 따른 해양 수질 및 퇴적물 영향평가 개선 방안)

  • Kim, Yeong-Tae;Kim, Gui-Young;Jeon, Kyeong-Am;Lee, Dae-In;Yu, Jun;Kim, Hee-Jung;Kim, In-Chul;Eom, Ki-Hyuk
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.19 no.2
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    • pp.119-128
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    • 2013
  • Since the early 2000s, demand for coastal dredging projects have been significantly increased, and the dredged sediments have showed the continuing marked increases through the multiple projects with other coastal development and constructions. As significant or potential degradation of marine environment has been mounting, we checked the current situation of marine environmental impact assessment through marine water and sediment qualities in relation with dredging projects of the sea area utilization consultation statements submitted in 2011. While analysis percentages of the general items were usually higher, harmful components such as metals revealed wide variation of analysis percentages. In the event of analysis of metals, the pre-treatment process (full digestion) and analysis method were not properly implemented in accordance with the guidelines for preparation of consultation statements. Although not specified in the guidelines, verification procedures (tests of recovery efficiency and detection limit) to secure the reliability were almost ignored. As a result, most of developers did conduct poor marine environmental impact assessment on coastal dredging and related projects. We suggested that the responsible government authority should establish new detailed guidelines on the sea area utilization consultation for more strict evaluation and diagnosis of marine environment and distinctly request the developer to obey the guidelines by complementing the system of the sea area utilization consultation.

Composition of Amino Acids, Minerals, and Heavy Metals in Differently Cooked Laver (Porphyra tenera) (김(Porphyra tenera)의 조리방법에 따른 아미노산, 무기질, 중금속 함량 분석)

  • Hwang, Eun-Sun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.8
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    • pp.1270-1276
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    • 2013
  • Laver, a red algae belonging to the genus Porphyra tenera, is one of the most widely consumed edible seaweeds in Korea, China, and Japan. Lavers are usually consumed in dried, roasted, and seasoned forms to improve their palatability. We evaluated the composition of amino acids, minerals, and trace heavy metals in these three differently cooked forms of laver. The moisture and ash contents of three differently cooked lavers ranged from 1.49~9.69% and 6.07~10.31%, respectively. The crude protein and lipid content ranged from 17.24~36.88% and 0.52~42.42%, respectively. Dried laver was found to be a good source of amino acids such as taurine, alanine, and glutamic acid (871.10 mg, 833.53 mg, and 719.77 mg per 100 g dry weight, respectively). Laver was a good source of macro and micro minerals such as K, Ca, Mg, Na, P, I, and Fe, although laver more extensively cooked (roasted and seasoned) contained less minerals compared to the dried form. Mercury levels in the three differently cooked forms of laver were all less than 100 ng/g dry weight (the limit of detection with our methodology). The levels of arsenic were the most abundant elements in the differently cooked laver. There was a clear variation, depending on the cooking process, in terms of amino acid, mineral, and trace metal contents of laver.

A Study on Migration of Ethylenediamine and Hexamethylenediamine from Polyamide Utensils (Polyamide 조리기구로부터 Ethylenediamine 및 Hexamethylenediamine의 이행에 관한 연구)

  • Eom, Mi-Ok;Kwak, In-Shin;Yoon, Hae-Jung;Jeon, Dae-Hoon;Choi, Hyun-Chul;Kim, Hyung-Il;Sung, Jun-Hyun;Park, Na-Young;Kim, So-Hee;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
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    • v.25 no.1
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    • pp.36-42
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    • 2010
  • The method for the determination of ethylenediamine (EDA) and hexamethylenediamine (HMDA) in food simulants was developed, and migration amounts of these compounds was monitored for 124 polyamide (PA) utensils. The diurethane derivatives of EDA and HMDA, which produced by reaction with ethyl chloroformate, were analyzed by using gas chromatograph (GC)/flame ionization detector (FID) and GC/mass spectrometer (MS). The developed method was validated with $0.3\;{\mu}g/mL$ of limit of detection (LOD) for EDA and $0.1\;{\mu}g/mL$ of LOD for HMDA, > 0.999 of linearity($r^2$) and > 88% of recovery. The EDA was detected 1.31 and $02.06\;{\mu}g/mL$ for 2 samples in water. The HMDA was detected $0.29\;-\;0.93\;{\mu}g/mL$ for 3 samples in 20% ethanol and $0.26\;-\;0.44\;{\mu}g/mL$ for 10 samples in n-heptane. These migration levels were below the specific migration limits (SML) of $12\;{\mu}g/mL$ and $2.4\;{\mu}g/mL$ for EDA and HMDA established in EU.

Investigation of Microbial Contamination in Semisulcospira libertine and Evaluation of Its Reduction Effects by Sediment Removal Treatment (다슬기(Semisulcospira libertine)의 미생물 오염도 평가 및 해감 제거공정에 따른 저감화 효과)

  • Choi, Man-Seok;Jun, Eun Bi;Choi, Seungho;Bang, Hyeon-Jo;Park, Shin Young
    • Journal of Food Hygiene and Safety
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    • v.34 no.4
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    • pp.361-366
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    • 2019
  • In this study, microbial contamivation semisulcospira libertine and effect of sedimentation treatment of major bacterial and fungal pathogens were investigated. The total aerobic bacteria, coliforms, Escherichia coli, Staphylococcus aureus, and yeast and mold present in raw and water-dipped Semisulcospira libertine were enumerated using the standard plate count methods on using the standard plate method on potato dextrose agar (PDA), 3M Petrifilm for coliforms / E. coli, 3M Petrifilm for S. aureus, and plate count agar (PCA), respectively. In analysis of microbial contamination of raw Semisulcospira libertine, the total aerobic bacteria, coliforms, and yeast and mold were monitored as 6.40, 2.70, and $6.79{\log}_{10}CFU/g$, respectively. Both E. coli and S. aureus were not detected (detection limit: 10 CFU/g). However, Semisulcospira libertine dipped in ground water for 3 hours had higher contamination levels of all natural indigenous microorganisms than raw Semisulcospira libertine. Especially, E. coli was detected as $2.46{\log}_{10}CFU/g$ in the ground water-dipped Semisulcospira libertine. The total aerobic bacteria in the ground water-dipped Semisulcospira libertine was not significantly reduced (p>0.05) compared to that in the raw Semisulcospira libertine. Moreover, coliforms were significantly increased (p>0.05) in all water-dipped Semisulcospira libertine. Only fungi were slightly reduced (less than 0.2 log) (p>0.05) in the tap water-dipped Semisulcospira libertine by comparison with the raw Semisulcospira libertine. The results of this study suggest that the use of chemical sterilizing agents and other physical methods in the washing stage will be necessary for the microbial reduction in raw Semisulcospira libertine because the use of sediment removal treatment by ground or tap water did not affect the microbiological safety of the raw Semisulcospira libertine.

Analytical Method for Determination of Laccaic Acids in Foods with HPLC-PDA and Monitoring (식품 중 락카인산 성분 분리정제를 통한 분석법 확립 및 실태조사)

  • Jae Wook Shin;Hyun Ju Lee;Eunjoo Lim;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.390-401
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    • 2023
  • Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r2=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.263-268
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    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.