• Title/Summary/Keyword: Spectrophotometry

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Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

Comparison of Standard and Lend Limit Test of Various Institutes on Lead Limit of Synthetic and Natural Food Additives (합성 및 천연 식품첨가물의 납함량에 대한 여러 기관의 규격기준 및 납시험법 비교)

  • Shin Dong-Hwa;Kim Yong-Suk;Jeong Do-Yeong;Lee Young-Hwan;Bang Jeong-Ho;Om Ae-Son;Shin Jae-Wook;Lee Tal-Soo;Jang Young-Mi;Hong Ki-Hyoung;Park Sung-Kwan;Park Sung-Kug;Kwon Yong-Kwan
    • Journal of Food Hygiene and Safety
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    • v.21 no.2
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    • pp.82-91
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    • 2006
  • Standard and lead limit test in general test method of Korea, Japan, Joint FAO/WHO Expert Committee of Food Additives (JECFA), USA, and EU on synthetic and natural food additives were compared. There were found that the general test methods in 'Korea Food Additives Code' were different from standards of various institutes on lead limit test. For the lead limit test of food additives, Korea used dithizone method, Japan used atomic absorption spectrophotometry, and USA used dithizone method, flame atomic absorption spectrophotometric method, atomic absorption spectrophotometric graphite furnace method, and APDC extraction method. In addition, JECFA and EU used dithizone method and atomic absorption spectrophotometric method. The dithizone methods of Korea, USA, and JECFA were nearly identical. In the case of USA, JECFA, and EU, the analytical methods for lead limit test were shown in individual monograph. Lead limit test against 13 synthetic, such as magnesium stearate and L-cystine, and 12 natural, such as gua gum and diatomaceous earth, food additives distributed in Korea were performed by the analytical method of each institute. Although all institutes use various methods for analysis of lead, contents of lead in food additives tested fell into the standard of each institute.

Factors Related to Poor School Performance of Elementary School Children (국민학교아동의 학습부진에 관련된 요인)

  • Park, Jung-Han;Kim, Gui-Yeon;Her, Kyu-Sook;Lee, Ju-Young;Kim, Doo-Hie
    • Journal of Preventive Medicine and Public Health
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    • v.26 no.4 s.44
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    • pp.628-649
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    • 1993
  • This study was conducted to investigate the factors related to the poor school performance of the elementary school children. Two schools in Taegu, one in the affluent area and the other in the poor area, were selected and a total of 175 children whose school performance was within low 10 percentile (poor performers) and 97 children whose school performance were within high 5 percentile (good performers) in each class of 2nd, 4th and 6th grades were tested for the physical health, behavioral problem and family background. Each child had gone through a battery of tests including visual and hearing acuity, anthropometry (body weight, height, head circumference), intelligence (Kodae Stanford-Binet test), test anxiety (TAI-K), neurologic examination by a developmental pediatrician and heavy metal content (Pb, Cd, Zn) in hair by atomic absorption spectrophotometry. A questionnaire was administered to the mothers for prenatal and prenatal courses of the child, family environment, child's developmental history, and child's behavioral and learning problems. Another questionnaire was administered to the teachers of the children for the child's family background, arithmatic & language abilities and behavioral problem. The poor school performance had a significant correlation with male gender, high birth order, broken home, low educational and occupational levels of parents, visual problem, high test anxiety score, attention deficit hyperactivity disorder (ADHD), poor physical growth (weight, height, head circumference) and low I.Q. score. The factors that had a significant correlation with the poor school performance in multiple logistic regression analysis were child's birth order (odds ratio=2.06), male gender(odds ratio=5.91), broken home(odds ratio=9.29), test anxiety score(odds ratio=1.07), ADHD (odds ratio=9.67), I.Q. score (odds ratio=0.85) and height less than Korean standard mean-1S.D.(odds ratio=11.12). The heavy metal contents in hair did not show any significant correlation with poor school performance. However the lead and cadmium contents were high in males than in females. The lead content was negatively correlated with child's grade(P<0.05) and zinc was positively correlated with grade (P<0.05). among the factors that showed a significant correlation with the poor school performance, high birth order, short stature and ADHD may be modified by a good family planning, good feeding practice for infant and child, and early detection and treatment of ADHD. Also, teacher and parents should restrain themselves from inducing excessive test anxiety by forcing the child to study and over-expecting beyond the child's intellectual capability.

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Mitigation of Calcification in Bovine Pericardial Bioprosthesis after Amino Acids Posttreatment (아미노산 후처치의 이종 심낭보철편 석회화 완화 효과)

  • 안재호
    • Journal of Chest Surgery
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    • v.36 no.3
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    • pp.131-135
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    • 2003
  • Bovine pericardium fixed in glutaraldehyde solution (GA) has been one of the most popular surgical bioprosthesis, however, late calcific degeneration after implantation remains to be solved. To mitigate calcific degeneration, we posttreated the bovine pericardium with amino acids after GA fixation. Material and Method: 40 small pieces of bovine pericardia were fixed in 0.625% GA solution with 4 g/L $MgCl_26H_2O$as a control group (group 1). 40 pieces fixed in the same GA solution were posttreated with 2% chitosan solution (group 2) and the other 40 pieces posttreated with 8% glutamate (group 3). These were implanted into the belly of forty Fisher 344 rats subdermally and extracted at f month, 2 months, 3 months and 4 months after implantation. Result: With atomic absorption spectrophotometry we measured the deposited calcium amount and the results were as follows; 2.01 $\pm$0.13 mg/g in group 1, 2.34$\pm$0.73 mg/g in group 2, 2.49$\pm$0.15 mg/g in group 3 at 1 month after implantation, and 3.57$\pm$0.15 mg/g in group 1, 3.52$\pm$0.92 mg/g in group 2, 3.46$\pm$0.12 mg/g in group 3 at the second month. But 5.45$\pm$0.42 mg/g in group 1, 3.22 $\pm$1.31 mg/g in group 2 and 4.20$\pm$0.55 mg/g in group 3 at the 3rd month, which have statistical significance in group 2 (p<0.05). Finally at 4th month, 6.01$\pm$1.21 mg/g in group 1, 3.78$\pm$1.82 mg/g in group 2, 3.92$\pm$0.92 mg/g in group 3, which also have statistical significance (p < 0.05). Conclusion: This means posttreatment with 2% chitosan shows meaningful calcium mitigation effects after 3rd month on subcutaneously implanted bovine pericardium in the rat models but 8% glutamate shows mitigation effect after 4months in this experiment.

Time Cource Variation of Metatarsus Mineral Content after UV Exposure to Dorsal Skin of Broiler Chicks (브로일러 병아리의 등 피부에 자외선 조사후 중족골 무기물 함량의 경시적 변화)

  • 장윤환;강훈석;김강수;원지웅
    • Korean Journal of Poultry Science
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    • v.19 no.1
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    • pp.35-45
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    • 1992
  • This study was carried out to investigate the effect of different dose of 312nm UV irradiation on ash and phosphorus contents in metatarsus of broiler chicks, whose dorsal skins were exposed to the UV light. Day old Hubbard line broiler chicks were fed with vitamin D deficient diet for 3 weeks and the defeathered dorsal skins were exposed to different dise (0.32, 0.65, or 0.98 J/$\textrm{cm}^2$) of 312nm UV light. The metatarsus bones were collected on 0, 1, 2, 3, 4 or 5 days after irradiation and defatted, dried, ashed and dissolved in 6N-HCI. The P concentrations were determined by spectrophotometry. When the 0.32 J/$\textrm{cm}^2$ dose was applied, the ash contents in metatarsus bones o( chicks were 42, 46 and 40% on 0, 1 and 3 days after irradiation, respectively. The maximum level, 46% was appeared at 2 days after exposure as 0.65 J/$\textrm{cm}^2$ was treated. When 0.98 J/$\textrm{cm}^2$ irradiation was applied, the high concentrations, 47 and 47% were shown on 1 and 2 days after irradiation, respectively. The 0.98 J/$\textrm{cm}^2$ among three levels of dose increased the most amount of ash in metatarsus bone. In respect to the P content in the chick bone the increased level, 19.4% was shown on 3 days after UV treatment with 0.32 J/$\textrm{cm}^2$. The maximum levels, 18.1 and 20.0% were present on 3 and 2 days after exposure to the 0.65 and 0.98 J/$\textrm{cm}^2$ of UV dose, respectively. It was shown that the higher dose of UV irradiation increased the more P concentration in matatarsus of chicks and the production rate was faster than those from 0.32 and 0.65 J/$\textrm{cm}^2$ treatments.

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Variation of Cadmium and Zinc Content in Paddy Soil and Rice from the Janghang Smelter Area (장항제련소 지역의 토양과 수도체중 Cd 및 Zn 함량의 변화)

  • Kim, Seong-Jo;Baek, Seung-Hwa
    • Korean Journal of Environmental Agriculture
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    • v.13 no.2
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    • pp.131-141
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    • 1994
  • To investigate differences in Cd and Zn contents in paddy soils and rice plants polluted by aerial emissions from the Janghang smelter, soil samples in the different directions and at the surface (0-15cm) and subsurface (15-30cm) in 1982 and 1990, and rice plants at the corresponding sampling sites in 1990 were collected from the Janghang Smelter Area. Soil samples were extracted with $4M-HNO_3$ and plant samples were digested with a mixture of $HNO_3$ and $HClO_4$for analyzing by atomic absorption spectrophotometry. The Cd and Zn contents in soils ranged from 0.09 to 4.42 and from 16.0 to 959.5mg $kg^{-1}$, respectively. The average contents of Cd and Zn in 1990 were higher than those in 1982. The Cd and Zn contents of soils near the center of the smelter were higher than those of soils farther from the center and also decreased in the order of east > north-north east > north east > north. The Cd and Zn levels in surface soils were higher than those in subsurface soils. The contaminated areas of Cd and Zn were within 4km in the east, and within 3km in the north-north east and the north east. Metal contents in brawn rice were the lowest in rice plants. The Cd content of brown rice was one sixth of that in leaf blade and in leaf sheath. The Cd content of leaf blade, stem and panicle axis were significantly correlated with the levels of Zn, Cu and Pb in soils, and Zn content of stem was significantly correlated with the levels of Cu and Pb. The Cd and Zn content in brown rice ranged from 0.05 to 0.25mg $kg^{-1}$ and from 10.5 to 30.9㎎ $kg^{-1}$ in the smelter area, respectively.

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Variation of Cadmium and Zinc Content in Rice and Soil of the Mangyeong River Area (만경강 유역의 토양과 수도체중 Cd 및 Zn 함량의 변화)

  • Kim, Seong-Jo;Baek, Seung-Hwa;Kim, Un-Sung;Yoon, Ki-Woun;Moon, Kwang-Hyun;Kang, Gyeong-Won
    • Korean Journal of Environmental Agriculture
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    • v.13 no.2
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    • pp.142-150
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    • 1994
  • To investigate differences in Cd and Zn contents of paddy soils and rice plants polluted by the municipal and industrial waste water in the Mangyeong River Area, soil and plant samples were collected at several distances from the main inlet and at different depths of the soil. Soil samples were extracted with $4M-HNO_3$ and plant samples were digested with a mixture of $HNO_3$and $HClO_4$for analyzing heavy metals by atomic absorption spectrophotometry. The contents of Cd and Zn in soils ranged from 0.38 to 1.17 and from 33.8 to 464.6mg kg^{-1}, respectively. The average Cd level in 1990 was less than that in 1982, but the Zn level in 1990 was higher than that in 1982 in general. No variation in Cd contents was observed in soils at the different distances from the source of waste water, but Zn contents in soils were lower with the increasing distances from the source of waste water. A significant correlation was observed among Cd content, OM, available silicate, CEC and $Ca^{++}$. Similar results existed among Zn content of 1982, OM and $Ca^{++}$. The Cd content in subsurface soils of 1992 was significantly correlated with Zn, Cu, and Pb in soils, and the Zn content in soils was significantly correlated with the Cu and Pb in soils, regardless of years. The Cd content in leaf blades of rice was more than seven times higher than that in brown rice. The Zn content in rice was higher than that in leaf blades and in panicle axis. The Cd content in panicle axis and the Zn content in all parts of rice were correlated with Zn, Cu and Pb contents in soils. The Cd and Zn contents in brown rice ranged from 0.10 to 0.90mg $kg^{-1}$ and from 4.2 to 95.9mg $kg^{-1}$ in the Mangyeong River Area, respectively.

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Antioxidant and Tyrosinase Inhibitory Effects of Brassica oleracea L. Fractions (적채 분획물의 항산화 및 Tyrosinase 억제 효과)

  • 윤경아;박윤자;배송자
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.1
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    • pp.7-15
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    • 2004
  • This research was designed to investigate the antioxidant activity of red cabbage (Brassica oleracea L., BO) fractions on the liposomes consisted of L-$\alpha$-dilinoleoylphosphatidylcholine (DLPC-liposome) and the tyrosinase activity of BO fractions. The methanol extract of BO (BOM) was fractionated into five different partition layers: hexane (BOMH), ethylether (BOMEE), ethylacetate (BOMEA), butanol (BOMB) and aqueous (BOMA) layers. The antioxidant activities of BOM fractions toward oxidized DLPC-liposome were examined by spectrophotometry measuring oxidized conjugated dines. The antioxidant activities of BOMEE and BOMEA fractions toward oxidized DLPC-liposomes were similar to the antioxidant activities of $\alpha$-tocopherol and weaker than that of BHT. The synergy effects of antioxidation of BOMEE and BOMEA fractions added with vitamin C and $\alpha$-tocopherol had even stronger antioxidant activities than the fractions without vitamin C and $\alpha$-tocopherol. These results showed that the fractions of BOMEE and BOMEA could be developed as a potent antioxidant. Out of five different partition layers of BOM fractions, BOMEA exhibited the strongest tyrosinase activity of 94% at a concentration of 40 $\mu\textrm{g}$/mL. This result suggests BOMEA fractions inhibit the foramation of melanin and therefore can be used as the inhibitor of melanin synthesis. Results of antioxidant activity and tyrosinase inhibition indicate that useful bioactive substances exist in BOMEE and BOMEA fractions. Both fractions from BO (red cabbage) have the potential of being developed into health related products.

A Comparison of Gases and Heavy Metals in Blood between Urban and Rural Teenager (도시(都市)와 농촌(農村) 약년자(若年者)의 혈액(血液)가스 및 중금속(重金屬) 함량(含量) 비교(比較))

  • Lee, Sang-Sook;Kim, Doo-Hie
    • Journal of Preventive Medicine and Public Health
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    • v.18 no.1
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    • pp.129-136
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    • 1985
  • This paper is carried out to determine the venous blood gas components and heavy metals, such as lead, cadmium and copper, in blood between urban and rural teenager. The subjects were 34 in urban, Taegu city and 37 in rural, Euisung-Gun. But smokers were excluded. The specimens were sampled in May, 1985. The heavy metals were analyzed by atomic absorption spectrophotometry (IL. 551) and carboxy-Hb, Met-Hb, Hb, $O_2\;and\;CO_2$, blood gas analyzer (IL. 1301) and CO-oximeter (IL. 282). In urban group, $PO_2\;and\;O_2-Hb$ were significantly lower than in rural (p<0.01, p<0.03, respectively), and ${HCO_3}^{-}\;and\;TCO_2$ were significantly higher than in rural (p<0.01, p<0.01, respectively). CO-Hb concentration was rather higher in the rural group than the urban (p<0.03), other Met-Hb was higher in urban group than in the rural (p<0.01). Lead and cadmium were also significantly higher in the urban group (p<0.03, p<0.02, respectively).

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Kinetics and Mechanism of Alkalie Hydrolysis of Cinnamonitrile (II) (Cinnamonitrile의 알카리 가수분해(加水分解) 반응(反應)메카니즘 (II))

  • Sung, Nack Do;Chung, Woo Jin;Kwon, Ki Sung;Park, Byung Kwan
    • Korean Journal of Agricultural Science
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    • v.10 no.2
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    • pp.354-364
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    • 1983
  • Confonmation of (Z)-cinnamonitrile have been studied by molecular orbital theoretically using extended Huckel theory(EHT) and CNDO/2 molecular orbital calculation methods. The results indicate that the stability of conformation is(Z)-gauch>(Z)-planar. The rate constants for alkalie hydrolysis of cinnamonitrile at pH 7.0-14.0 range have been determined by ultra-violet spectrophotometry in 50% methanol at $25^{\circ}C$ and the following rate equation which can be applied over wide pH range was obtained; $${\therefore}k=({\frac{1.41{\times}10^{-14}+1.21{\times}10^7/[H_3O^+]}{2.65{\times}10^{-7}+1.64/[H_3O^+]})+9.14{\times}10^9/[H_3O^+]$$ The rate equation reveals that, at pH 7.0-10.0, the reaction is initiated by the addition of water molecule to unsaturated cabon-carhon double bond of cinnamonitrile and ${\alpha}C-{\beta}C$ bond scission follow subsequently in neutral and alkalie media. At pH 12.0-14.0, in strong alkalie solution, that so-called Michael type nucleophilic addition that the over-all rate constants is only dependent upon the concentration of hydroxide ion occurs competitively and are very complicated. Hence, the reaction mechanism of alkalie hydrolysis of cinnamonitrile which did not carefully before can be fully explained.

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