• Title/Summary/Keyword: high-performance liquid chromatography

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Validation of an Analytical Method for Deacetylasperulosidic acid, Total Sugar and Monosaccharide Analysis in Fermented Morinda citrifolia Polysaccharide Powder (발효노니 다당체 분말의 deacetylasperulosidic acid, 총당 및 단당류 분석법 검증)

  • Kwon, Heeyeon;Choi, Jisoo;Kim, Soojin;Kim, Eunmin;Uhm, Jihyun;Kim, Bokyung;Lee, Jaeyeon;Kim, Yongdeok
    • Journal of Food Hygiene and Safety
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    • v.37 no.4
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    • pp.216-224
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    • 2022
  • This study was aimed at validating the analysis methods for deacetylasperulosidic acid (DAA), total sugar, galacturonic acid, glucose, and galactose, which are the indicator components of fermented Morinda citrifolia polysaccharide extract (Vitalbos). We modified the previously reported methods for validating the analytical methods. The specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) were measured using phenol-sulfuric acid method and high-performance liquid chromatography (HPLC). The retention time and spectrum of the standard solution of Vitalbos coincided, confirming the specificity. The calibration curve correlation coefficient (R2), of five indicator components, ranged from 0.9995-0.9998, indicating excellent linearity of 0.99 or more. The intra-day and inter-day precision range of the assay was 0.14-3.01%, indicating a precision of less than 5%. The recovery rate was in the range of 95.13-105.59%, presenting excellent accuracy. The LOD ranged from 0.39 to 0.84 ㎍/mL and the LOQ ranged from 1.18 to 2.55 ㎍/mL. Therefore, the analytical method was validated for DAA, total sugar, galacturonic acid, glucose, and galactose, in Vitalbos. The indicator component content in Vitalbos was determined using a validated method. The contents of DAA, total sugar, galacturonic acid, glucose, and galactose were 2.31±0.06, 475.92±5.95, 72.83±1.05, 71.63±2.44, and 67.30±2.31 mg/g of dry weight, respectively. These results suggest that the developed analytical method is efficient and could contribute to the quality control of Vitalbos, as a healthy functional food material.

Anti-stress and Sleep-enhancing Effects of Ptecticus tenebrifer Water Extract Through the Regulation of Corticosterone and Melatonin Levels (코르티코스테론 및 멜라토닌 수치 조절을 통한 동애등에 물 추출물의 항스트레스 및 수면 개선 효과)

  • Oh, Dool-Ri;Ko, Haeju;Hong, Seong Hyun;Kim, Yujin;Oh, Kyo-Nyeo;Kim, Yonguk;Bae, Donghyuck
    • Journal of Life Science
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    • v.32 no.8
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    • pp.601-610
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    • 2022
  • P. tenebrifer (PT) belongs to the Diptera order and Stratiomyidae family. Recently, insect industry have been focused as food, animal feed and environmental advantages. γ-aminobutyric acid (GABA) and melatonin have been associated with regulating sleep and depression. GABA is the primary inhibitory neurotransmitter and is synthesized via biotransformation of monosodium glutamate (MSG) to GABA by lactic acid bacteria. In this study, we first used a GABA-enhanced PT extract, wherein GABA was enhanced by feeding MSG to PT. The underlying mechanisms preventing stress and insomnia were investigated in a corticosterone (CORT)-induced endoplasmic reticulum (ER) stress and chronic restraint stress (CRS)-exposed mouse model, as well as in pentobarbital (45 mg/kg)-induced sleep behaviors in mice. In the present study, the GABA peak was detected in high-performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) analysis and showed in Ptecticus tenebrifer water extract (PTW) but not in non-PTW extract. The results showed that PTW and Ptecticus tenebrifer with 70% ethanol extract (PTE) exerted neuroprotective effects by protecting against CORT-induced downregulation of phosphorylated extracellular signal-regulated kinase 1/2 (ERK1/2) and cAMP-response element binding protein (CREB) expression. In addition, PTW (300 mg/kg) significantly reduced CORT levels in CRS-exposed mice. Furthermore, PTW (100 and 300 mg/kg) significantly reduced sleep latency and increased total sleep duration in pentobarbital (45 mg/kg)-induced sleeping behaviors, which was related to serum melatonin levels. In conclusion, our results suggest that PTW exerts anti-stress and sleep-enhancing effects by regulating serum CORT and melatonin levels.

Studies on Xylooligosaccharide Analysis Method Standardization using HPLC-UVD in Health Functional Food (건강기능식품에서 HPLC-UVD를 이용한 자일로올리고당 시험법의 표준화 연구)

  • Se-Yun Lee;Hee-Sun Jeong;Kyu-Heon Kim;Mi-Young Lee;Jung-Ho Choi;Jeong-Sun Ahn;Kwang-Il Kwon;Hye-Young Lee
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.72-82
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    • 2024
  • This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C18 column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.

Evaluation of Neonicotinoid Pesticides' Residual Toxicity to Honeybees Following or Foliage Treatment (네오니코티노이드계 농약의 사용방법에 따른 꿀벌엽상잔류 독성 평가)

  • Jin Ho Kim;Chul-Han Bae;ChangYul Kim
    • Journal of the Korean Applied Science and Technology
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    • v.41 no.2
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    • pp.484-497
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    • 2024
  • Neonicotinoid pesticides, widely used worldwide as potent insecticides, have been found to have detrimental effects on the environment and living organisms due to their persistent residues. This study aimed to investigate the neonicotinoid pesticides, imidacloprid, and clothianidin, focusing on their impact on honey bee toxicity and foliar residue levels. Alfalfa was selected as control crop while bell peppers, and cucumbers were chosen as representative application crops, respectively. The investigation involved comparing the toxicity and foliar residue levels resulting from soil and foliar treatments, with a focus on identifying potential shortcomings in conventional foliar residue toxicity testing methods. Imidacloprid and clothianidin were applied to crops or soil at recommended rates and through irrigation. The honey bee mortality rate (RT25) over time was determined, and pesticide residues on leaves were quantified using High-Performance Liquid Chromatography (HPLC). The results revealed that foliar treatment with imidacloprid on alfalfa resulted in an RT25 of less than 1 day, with residues ranging from 1.07 to 19.27 mg/kg. In contrast, application on bell peppers showed RT25 within 9 days, with residues ranging from 1.00 to 45.10 mg/kg. Clothianidin foliar treatment displayed RT25 within 10 days on alfalfa, with residues between 0.61 and 2.57 mg/kg. On bell peppers, RT25 was within 28 days, with residues ranging from 0.13 to 2.85 mg/kg. Soil treatment with imidacloprid and clothianidin in alfalfa exhibited minimal impact on honey bees and residues of 0.05 to 0.37 mg/kg. However, in applied crops, imidacloprid showed RT25 within 28 days and residues ranging from 4.47 to 130.43 mg/kg, while clothianidin exhibited RT25 within 35 days and residues between 5.96 and 42.32 mg/kg. In conclusion, when comparing honey bee toxicity and foliar residues among crops, application crops had a more significant impact on honey bee mortality and higher residue levels compared to control crops. Moreover, soil treatment for application crops resulted in higher RT25 and residue levels compared to foliar treatment. Therefore, to ensure pesticide safety and environmental sustainability, diverse research approaches considering different crops and application methods are necessary for the safety assessment of imidacloprid and clothianidin.

The Changes of Plasma Catecholamines Concentration during Waking and Sleep in Obstructive Sleep Apnea Syndrome Patients with Systemic Hypertension (전신성 고혈압을 동반한 폐쇄성 수면 무호흡증후군 환자에서 각성시와 수면중의 혈장 Catecholamines 농도 변화)

  • Moon, Hwa Sik;Lo, Dae Guen;Choi, Young Mee;Kim, Young Kyoon;Kim, Kwan Hyoung;Song, Jeong Sup;Park, Sung Hak
    • Tuberculosis and Respiratory Diseases
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    • v.43 no.4
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    • pp.600-612
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    • 1996
  • Background : Recent studies deported that untreated patients with obstructive sleep apnea syndrome had high long-term mortality rates, and cardiovascular complications of these patients clad a major effect on mortality. Several data indicates that obstructive sheep apnea syndrome contributes to the development of diurnal systemic hypertension. But the pathophysiological mechanism of the development of systemic hypertension in these patients is still uncertain. This study was performed to evaluate the possible role of sympathetic nervous system activity for the development of systemic hypertension in patients with obstructive sleep apnea syndrome. Method : 35 patients with obstructive sleep apnea syndrome(OSAS) and 13 Control subjects(control) were included in this study. 21 patients of OSAS were normotensives(OSAS-NBP), and 14 patients of OSAS were hypertensives(OSAS-HBP). Full night polysomnography was undertaken to all subjects. We measured plasma norepinephrine(NE) and epinephrine(EP) concentrations during waking and sleep, using high performance liquid chromatography, in all patients and control subjects. Results : In OSAS, OSAS-NBP and control, plasma NE and EP concentrations during sleep were lowed than during waking(p<0.01). But, in OSAS-HBP, these was no difference between during waking and sleep. Plasma NE concentrations during sleep of OSAS, OSAS-NBP and OSAS-HBP were higher than Control(p<0.05). In OSAS-HBP, daytime systolic blood pressure correlated with plasma NE concentration during sleep(r=0.7415, p<0.01), arid correlated inversely with mean arterial oxygen saturation(r=-0.6465, p<0.05) or arterial oxygen saturation nadir(r=-0.6) 14, p<0.05) during sleep. Conclusion : The sympathetic activity during sleep of obstructive sleep apnea syndrome patients was higher than control subjects. In obstructive sleep apnea syndrome patients with systemic hypertension, there was no diurnal variation of sympathetic activity, and there was correlation between daytime systolic blood pressure and sympathetic activity during sleep. These data suggests that chronic hyperactivity of sympathetic nervous system may contribute to the development of diurnal systemic hypertension in patients with obstructive sleep apnea syndrome.

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Review of Sexual Dysfunction in Male Schizophrenics (남자 정신분열병 환자에서 성기능장애에 대한 검토)

  • Choi, Yeong Tae;Cheon, Jin Sook;Oh, Byoung Hoon
    • Korean Journal of Biological Psychiatry
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    • v.7 no.1
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    • pp.85-98
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    • 2000
  • Objective : There are four possible explanations for the sexual dysfunction of schizophrenics. The first is the possibility of a real structural aspect. The second possibility is that sexual function changes secondary to the illness. The third possibility is that there are medical and sociocultural barriers to sexual expression for chronic schizophrenics. The fourth possibility is that sexual dysfunction due to antipsychotic medication. However, we didn't know the precise cause of sexual dysfunction in schizophrenics. Therefore, the purpose of this study was to explore the mechanism of illness itself and antipsychotics on sexual dysfunction in male schizophrenics. Methods : The serum prolactin(PRL), testosterone(TST), and the plasma serotonin(5-HT) concentrations were measured by radioimmunoassay and high performance liquid chromatography method for 100 healthy male schizophrenics according to the DSM-IV. Concomitantly, the severity of psychotic symptoms using Clinical Global Impression(CGI), Brief Psychiatric Rating Scale(BPRS), Positive and Negative Syndrome Scale(PANSS), and the severity of side effects for antipsychotics using Extrapyramidal Side Effects Scale(EPSE), Anticholinergic Side Effects Scale(ACSE), the cognitive function using PANSS-Cognitive Function(PANSS-CF), Mini Mental State Exam-Korean(MMSE-K), and the sexual dysfunction using Sexual Functioning Questionnaire(SFQ), Questionnaire for Sexual Dysfunction in Men were assessed. The PRL, TST, and 5-HT levels of 50 healthy male controls who had no medical, neurological, and psychiatric illnesses were evaluated. The sexual function using SFQ(items FGa, FNa) were also assessed. Furthermore, the correlation with age, education, religion, economic status, age at onset, duration of illnesses, duration of admission, levels of PRL, TST, 5-HT, antipsychotic dosages, potency, benztropine, total duration of medication, EPSE, ACSE, CGI, BPRS, PANSS, PANSS-CF, MMSE-K and sexual dysfunctions were identified in male schizophrenics. Results : 1) The frequencies of sexual dysfunctions for schizophrenics(80%) were significantly(p<0.001) higher than those for controls(42%). The sexual dysfunctions according to sexual response cycle were 'low sexual desire' 76%, 'impairment of achieving erection' 75%, 'impairment of maintaining erection' 75%, 'impairment of obtaining orgasm' 32%, 'impairment in the quality of orgasm' 61%, 'impairment in quantity of ejaculate' 44%, 'premature ejaculation' 15%, and 'delayed ejaculation' 50%. 2) The PRL, 5-HT levels of schizophrenics($28.5{\pm}20.6ng/ml$, $298.5{\pm}89.1ng/ml$) were significantly(p<0.001) higher than those of controls($10{\pm}5.6ng/ml$, $169.2{\pm}37.8ng/ml$), while the TST levels of schizophrenics($4.3{\pm}1.5ng/ml$) and controls($4.5{\pm}1.2ng/ml$) were not significantly different. The sexual dysfunctions of schizophrenics who had abnormal 5-HT levels($4.7{\pm}1.3$ scores) were significantly(p<0.05) higher than those of who had normal 5-HT levels($3.8{\pm}1.6$ scores) on item D7. 3) The sexual dysfunctions of unmarried schizophrenics were significantly(p<0.01 : p<0.05) higher than those of married schizophrenics($6.1{\pm}2.8$ scores, $4.7{\pm}1.3$ scores on item FGa : ${\beta}$=-0.211 on item FNa). The sexual dysfunctions were positively correlated with the rise of 5-HT levels(r=0.209, p<0.05 on item D4 and r=0.241, p<0.05 on item D7), the higher age at onset(r=0.275, p<0.01 on item FNa : r=-0.202, p<0.05 on item FDa), the longer duration of illnesses(r=0.237, p<0.05 on item D6), the longer duration of admission(r=0.234, p<0.05 on item D4 : r=0.328, p<0.05 on item D6), the longer total duration of medication(r=0.237, p<0.05 on item D6). However, age, education, religion, economic status, PRL, TST levels, antipsychotics dosage, potency, benztropine, ACSE, CGI, BPRS, PANSS, PANSS-CF, MMSE-K scores were not correlated with increased sexual dysfunctions. Conclusions : Male schizophrenics have significantly more sexual dysfunction to compare with controls. The higher frequencies of sexual dysfunctions were low sexual desire and erectile disorder. The unmarried, higher age at onset, and longer duration of diseases were positively correlated with increased sexual dysfunctions. Also high 5-HT levels were positively correlated with increased sexual dysfunctions. This means that studies of plasma 5-HT levels, albeit questionable indicators of central 5-HT function, offer some additional support for the association of sexual dysfunction with excess 5-HT activity as primary pathology of schizophrenia. Our findings suggest that excess 5-HT activity seems to affect the patient's sexual function.

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A Monitoring of Aflatoxins in Commercial Herbs for Food and Medicine (식·약공용 농산물의 아플라톡신 오염 실태 조사)

  • Kim, Sung-dan;Kim, Ae-kyung;Lee, Hyun-kyung;Lee, Sae-ram;Lee, Hee-jin;Ryu, Hoe-jin;Lee, Jung-mi;Yu, In-sil;Jung, Kweon
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.267-274
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    • 2017
  • This paper deals with the natural occurrence of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in commercial herbs for food and medicine. To monitor aflatoxins in commercial herbs for food and medicine not included in the specifications of Food Code, a total of 62 samples of 6 different herbs (Bombycis Corpus, Glycyrrhizae Radix et Rhizoma, Menthae Herba, Nelumbinis Semen, Polygalae Radix, Zizyphi Semen) were collected from Yangnyeong market in Seoul, Korea. The samples were treated by the immunoaffinity column clean-up method and quantified by high performance liquid chromatography (HPLC) with on-line post column photochemical derivatization (PHRED) and fluorescence detection (FLD). The analytical method for aflatoxins was validated by accuracy, precision and detection limits. The method showed recovery values in the 86.9~114.0% range and the values of percent coefficient of variaton (CV%) in the 0.9~9.8% range. The limits of detection (LOD) and quantitation (LOQ) in herb were ranged from 0.020 to $0.363{\mu}g/kg$ and from 0.059 to $1.101{\mu}g/kg$, respectively. Of 62 samples analyzed, 6 semens (the original form of 2 Nelumbinis Semen and 2 Zizyphi Semen, the powder of 1 Nelumbinis Semen and 1 Zizyphi Semen) were aflatoxin positive. Aflatoxins $B_1$ or $B_2$ were detected in all positive samples, and the presence of aflatoxins $G_1$ and $G_2$ were not detected. The amount of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in the powder and original form of Nelumbinis Semen and Zizyphi Semen were observed around $ND{\sim}21.8{\mu}g/kg$, which is not regulated presently in Korea. The 56 samples presented levels below the limits of detection and quantitation.

Facile [11C]PIB Synthesis Using an On-cartridge Methylation and Purification Showed Higher Specific Activity than Conventional Method Using Loop and High Performance Liquid Chromatography Purification (Loop와 HPLC Purification 방법보다 더 높은 비방사능을 보여주는 카트리지 Methylation과 Purification을 이용한 손쉬운 [ 11C]PIB 합성)

  • Lee, Yong-Seok;Cho, Yong-Hyun;Lee, Hong-Jae;Lee, Yun-Sang;Jeong, Jae Min
    • The Korean Journal of Nuclear Medicine Technology
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    • v.22 no.2
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    • pp.67-73
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    • 2018
  • $[^{11}C]PIB$ synthesis has been performed by a loop-methylation and HPLC purification in our lab. However, this method is time-consuming and requires complicated systems. Thus, we developed an on-cartridge method which simplified the synthetic procedure and reduced time greatly by removing HPLC purification step. We compared 6 different cartridges and evaluated the $[^{11}C]PIB$ production yields and specific activities. $[^{11}C]MeOTf$ was synthesized by using TRACERlab FXC Pro and was transferred into the cartridge by blowing with helium gas for 3 min. To remove byproducts and impurities, cartridges were washed out by 20 mL of 30% EtOH in 0.5 M $NaH_2PO_4$ solution (pH 5.1) and 10 mL of distilled water. And then, $[^{11}C]PIB$ was eluted by 5 mL of 30% EtOH in 0.5 M $NaH_2PO_4$ into the collecting vial containing 10 mL saline. Among the 6 cartridges, only tC18 environmental cartridge could remove impurities and byproducts from $[^{11}C]PIB$ completely and showed higher specific activity than traditional HPLC purification method. This method took only 8 ~ 9 min from methylation to formulation. For the tC18 environmental cartridge and conventional HPLC loop methods, the radiochemical yields were $12.3{\pm}2.2%$ and $13.9{\pm}4.4%$, respectively, and the molar activities were $420.6{\pm}20.4GBq/{\mu}mol$ (n=3) and $78.7{\pm}39.7GBq/{\mu}mol$ (n=41), respectively. We successfully developed a facile on-cartridge methylation method for $[^{11}C]PIB$ synthesis which enabled the procedure more simple and rapid, and showed higher molar radio-activity than HPLC purification method.

Survey of Daily Caffeine Intakes from Children's Beverage Consumption and the Effectiveness of Nutrition Education (어린이들의 음료를 통한 카페인 섭취량 실태조사 및 영양교육에 따른 효과 평가)

  • Kim, Sung-Dan;Yun, Eun-Sun;Chang, Min-Su;Park, Young-Ae;Jung, Sun-Ok;Kim, Dong-Gyu;Kim, Youn-Cheon;Chae, Young-Zoo;Kim, Min-Young
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.6
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    • pp.709-720
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    • 2009
  • This study was conducted to identify daily caffeine intakes in beverages for elementary school children and to evaluate its effectiveness after nutrition education. The caffeine contents of 140 commercial beverages were analysed by high performance liquid chromatography-ultraviolet detector (HPLC-UV) and information about their consumption were obtained by surveying 267 children. Researchers gave nutrition education to the children, who were 6 to 11 years old and attended 9 classes of 3 elementary schools, by lecture, Powerpoint file and moving picture. Their preference and intake amount on beverages were investigated by questionnaire before and after nutrition education. The order on caffeine contents was coffee ($33.8{\pm}2.4{\sim}49.1{\pm}5.6\;mg/100\;mL$)> coffee milk ($10.6{\pm}3.3\;mg/100\;mL$)> cola ($6.0{\pm}2.4\;mg/100\;mL$)> green black oolong tea drink ($6.0{\pm}2.4\;mg/100\;mL$)> chocolate milk and chocolate drink ($1.6{\pm}0.7{\sim}1.7\;mg/100\;mL$)> black ice tea mix ($1.3{\pm}1.7\;mg/100\;mL$). The order on children's preference was carbonated drink and fruit and vegetable drink (27%)> sports drink (26%)> processed cocoa mix (7%)> milk (6%)> vitamin & functional drink (3%)> green tea drink (2%)> black tea drink and coffee (1%). The average daily caffeine intakes except tea drink was $5.9{\pm}11.2$ mg/person/day ($0.17{\pm}0.32$ mg/kg bw/day), ranged from $0.0{\sim}80.5$ mg/person/day for children. The sources of caffeine were coffee 57% (3.4 mg/person/day), coffee milk 20% (1.2 mg/person/day), carbonated drink 15% (0.9 mg/person/day), chocolate milk and chocolate drink 6% (0.4 mg/person/day), and vitamin & functional drink 2% (0.1 mg/person/day). After nutrition education, the preference of carbonated drink, coffee, vitamin drinks & functional drink was decreased significantly (p<0.05, p<0.05, p<0.01) and the intakes of carbonated drink, chocolate milk & chocolate drink, and vitamin & functional drink were also decreased significantly (p<0.01, p<0.05, p<0.01). This study has shown that nutrition education influences the preference and the intake behavior of caffeinated beverages.