• Title/Summary/Keyword: Assay error

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Liquid Chromatography-tandem Mass Spectrometry for Quantification of Dioscin in Rat Plasma

  • Kong, Tae Yeon;Ji, Hye Young;Choi, Sang-Zin;Son, Miwon;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • v.4 no.3
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    • pp.55-58
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    • 2013
  • Dioscin is a biologically active steroidal saponin with anticancer and hepatoprotective effects. A rapid, selective, and sensitive liquid chromatographic method with electrospray ionization tandem mass spectrometry was developed for the quantification of dioscin in rat plasma. Dioscin was extracted from rat plasma using ethyl acetate at acidic pH. The analytes were separated on a Halo C18 column using gradient elution of acetonitrile and 0.1% formic acid and detected by tandem mass spectrometry in selected reaction monitoring mode. The standard curve was linear ($r^2$ = 0.998) over the concentration range of 1-100 ng/mL. The lower limit of quantification was 1.0 ng/mL using 50 ${\mu}L$ of plasma sample. The coefficient of variation and relative error for intra- and inter-assay at four QC levels were 1.3 to 8.0% and -5.4 to 10.0%, respectively. This method was applied successfully to the pharmacokinetic study of dioscin after oral administration of dioscin at a dose of 29.2 mg/kg in male Sprague-Dawley rats.

Development of Differential Diagnosis and Treatment Method of Reproductive Disorders Using Ultrasonography in Cows II. Differential Diagnosis of Subestrous Dairy Cows (초음파검사에 의한 소의 번식장애 감별진단 및 치료법 개발 II. 무발정우의 감별진단)

  • 강병규;최한선;강현구;오기석;서동호;손창호;서국현
    • Journal of Veterinary Clinics
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    • v.15 no.2
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    • pp.307-318
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    • 1998
  • Accuracy of rectal palpation and ultrasonography for differential diagnosis of subestrous dairy trows were investigatedl using the result of pIRsma progesterone assay. The ovaries were examined 2 times of 10 days interval in 520 posearom and postinsemination subestroHs dairy cows, using rectal palpation and B-mode transrectal ultrasonography. The results of rectal palpation, ultrasonographic examination and measurement of plasma progesterone profiles in 520 subestrous dairy cows were silent brat or error of estrus detection 303 (58.3%), persistent corpus luteum 59 (11.3%), follicular cyst 37 (7.1%), luteal cyst 16 (3.1%), inactive ovary 9 (1.7%), granulosa tumor 1 (0.2%), hydmsalphinx 1 (0.2%), endomehris 81 (15.6%), pyometra 12 (2.3%) and mummified fetus 1 (0.2%), respectively. Accuncy of rectal palpation and ultrasonography for diagiosing ovarian disordeir based on plasma progesterone profiles were silent heat or error of estrus detection 80.5% and 96.7%$\boxUl$ persistent corpus luteum 57.6% and 94.9%, follicular cyst 62.5% and 91.9%1 luteal cyst 62.5% and 87.5%, maclive ovary 55.6% and 88.9% and granulosa cell tumor 100% and 100%, respectively. Acnuucy of rectal palpation for diagnosing uterine disorders based on ultrasonography was pyometra 75.0%1 endometritis 51.9% and mummified fetus 100%, respectively. Cbaracteristic ultrasonographic appearances of ovaries in subestrous dairy cows were as follows; Silent heat or error of estrus detection: anechoic follicle or hypoechoic corpus luteum than ovarian stroma was alternately present on Day 0 (first examination) and Day 10. Follicular cyst: uniformly nonechogenic ovarian structure $\geq $ 25 mm in diameter with a wall < 3 mm was present in ipsilateral on Day 0 and Day 10. Luteal cyst: luteal cyst was similar to follicular cysts but thickness of cystic wall was $\geq $ 3 mm. Inactive ovary : structures within ovaries was not present on Day 0 Bnd Day 10. Characteristic uthssonograpsc appearances of uterus in subestrous dairy cows were as follows; Endometritis: characterized by uterine lumen containing fluid in which 'snowy'echogenic particles art suspended. Pyometra: ultrasonographic appearance of pyometra was diffuse echogenic particles distributed in fluid within the distended uterus, and a thickened uterine wall. These results indicated that ultrasonography was practical far diagnosing reproductive disorders. To diagnosing ovarian disorders, ultrasonography should be carried out 2 times of 10 days interval and rndometritis should be differentiated with uterus of luteal phase in normal cycling cows.

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Comparison of the Correction Methods for Gamma Ray Attenuation in the Radioactive Waste Drum Assay (방사성폐기물드럼 핵종분석에서 감마선 감쇠보정 방법들의 비교 평가)

  • Ji Young-Yong;Ryu Young-Gerl;Kwak Kyoung-Kil;Kang Duck-Won;Kim Ki-Hong
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.4 no.3
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    • pp.275-284
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    • 2006
  • In the measurement of gamma rays emitted from the nuclide in the radioactive waste drum, to analyze the nuclide concentration accurately, it is necessary to use the proper calibration standards and to correct for the attenuation of the gamma rays. Two drums having a different density were used to analyze the nuclide concentration inside the drum in this study. After carrying out the system calibration, we measured the gamma rays emitted from the standard source inside the model drum with changing the distance between the drum and the detector. The measured values were corrected with the three kinds of gamma attenuation correction methode, as a results, the error was less than 10 % in the low density drum and less than 25 % in the high density drum. The measured activity in the short distance was more accruable than in the long distance. The transmission correction for the mass attenuation showed good results(very Low error) compared to the mean density and the differential peak correction method.

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Utilization of Near Infrared Spectroscopy for Analysis of Proximate Composition and Starch in Alaska Pollack Surimi (명태 수리미의 일반성분 및 전분의 분석을 위한 근적외선 분광분석법의 이용)

  • Song Ho Su;Lee Keun Tai;Park Seong Min;Hwang Sun Young
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.35 no.4
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    • pp.321-326
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    • 2002
  • Near infrared spectroscopy (NIR), is recently applied to analysis of food, and it gives non-destructive and highly reproducible results. The objectives of this study were to assay protein, lipid and starch content in Alaska pollack surimi and to investigate application in seafood. NIR spectra showed the absorbance signal at 1,510 nm, 2,050 nm, 2,170 nm and 2,180 nm for protein, and signal were increased with protein content. Standard error of equation (SEE) was 0,296 and standard error of prediction (SEP) was 0.327. In analysis of lipid in Alaska pollack surimi by NIR, near infrared spectra of lyophilized Alaska pollack surimi were scanned and the signals of absorbance from C-H functional groups in lipid were identified at 1,730 nm, 1,740 nm and 2,300 nm and these signals were risen as Increasing lipid contents of Alaska pollack surimi as samely protein. SEE and SEP were 0.319, 0,353, respectively. In starch analysis using NIR the signals of starch distinctly changed at wavelength of 1,450 nm and 1,950 nm. Collected values of SEE and SEP were 0.304 and 0.318, respectively and the range of errors was $0.0186\~0.6470$ in starch contents.

Vitamin C Tablet Assay by Near -Infrared Reflectance spectrometry

  • Kargosha, Kazem;Ahmadi, Hamid;Nemati, Nader
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.4111-4111
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    • 2001
  • When a drug is prepared in a tablet, the active component represents only a small portion of the dosage form. The other components of the formulation include materials to assist in the dissolution, antioxidants, coloring agents and bulk fillers. The tablets are tested using approved testing methods usually involving separation and subsequent quantification of the active component. Tablets may also be tested by near-Infrared Reflectance spectrometry (NIRS). In the present study, based on NIRS and multivariate calibration methods, a novel and precise method is developed for direct determination of ascorbic acid in vitamin C tablet. Two different tablet formulations were powdered in three different sizes, 63-125 ${\mu}{\textrm}{m}$, and examined. Spectral region of 4750-4950 $cm^{-1}$ / was used and optimized for quantitative operations. Partial least squares (PLS) and multiple linear regression (MLR) methods were performed for this spectral region. The results of optimized PLS and MLR methods showed that reproducibility increase with decreasing grain size and standard error of calibration (SEP) of less than 1% w/w of ascorbic acid and a correlation coefficient of 0.998 can be achieved. The PLS method showed better results than MLR. Seven overdose and underdose samples (prepared in the laboratory to match marketed products) were tested by proposed and iodometric standard methods. A correlation between NIRS predicted ascorbic acid values and iodomet.ic values was calculated ($R^2$=0.9950). Finally, the direct analysis of individual intact tablets in their unit-dose packages (Blistering in aluminum and PVC foils) obtained from market were also carried out and a correlation coefficient of 0.9989 and SEP of 0.931% w/w of ascorbic acid were achieved.

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Determination of Tiapride in Human Plasma Using Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

  • Moon, Ya;Paek, In-Bok;Kim, Hui-Hyun;Ji, Hye-Young;Lee, Hye-Won;Park, Hyoung-Geun;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • v.27 no.9
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    • pp.901-905
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    • 2004
  • A rapid, sensitive and selective hydrophilic interaction liquid chromatography-tandem mass spectrometric(HILIC-MS/MS) method for the determination of tiapride in human plasma was developed. Tiapride and internal standard, metoclopramide were extracted from human plasma with dichloromethane at basic pH and analyzed on an Atlantis HILIC silica column with the mobile phase of acetonitrile-ammonium formate (190 mM, pH 3.0) (94:6, v/v). The ana-Iytes were detected using an electrospray ionization tandem mass spectrometry in the multi-ple-reaction-monitoring mode. The standard curve was linear (r=0.999) over the concentration range of 1.00-200 ng/mL. The coefficient of variation and relative error for intra- and inter-assay at three QC levels were 6.4∼8.8% and -2.0∼3.6%, respectively. The recoveries of tiapride ranged from 96.3 to 97.4%, with that of metoclopramide (internal standard) being 94.2%. The lower limit of quantification for tiapride was 1.00 ng/mL using 1 00 $\mu$L of plasma sample.

Study on Metabolism and Excretion of Carteolol in Human Urine using GC/MS (GC/MS를 이용한 carteolol의 대사 및 배설연구)

  • Min, Hye-Ki;Kim, Myungsoo;Cho, Hyun-Woo;Kim, Taek-Jae;Kim, Dong-Hyun;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.482-487
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    • 2002
  • International Olympic Committee (IOC) prohibits the use of carteolol which is one of ${\beta}$-blockers. To prove whether carteolol product was taken or not, the analytical method in urine using GC/MS was established, and metabolism and excretion study were evaluated. As compared with acid hydrolysis, enzyme hydrolysis method was more efficiency. Coefficients of variation for intra-assay precision was around 10%. Error was less than 5% except the concentration of $0.05{\mu}g/m{\ell}$. Recovery was 78.5% at $2{\mu}g/m{\ell}$. Free carteolol, conjugated carteolol, and small amount of p-OH carteolol were found in dosed human urine samples. The conjugated form was being 59.4% of the total carteolol in human urine. The amount of carteolol renal excreted for 72 h after oral dose of 10 mg of carteolol was 49% of the administred dose.

Reproductive Monitoring and Estrus Induction using Ultrasonography and Hormone Assay in Dairy Cows I. Periodical Examination of Reproductive Status and Treatment of Reproductive Dysfunctions (초음파검사 및 호르몬검사에 의한 젖소 번식검진과 발정유도 I. 정기적인 번식검진 및 번식장애 치료)

  • 오기석;박상국;김방실;고진성;신종봉;백종환;홍기강;문광식;임원호
    • Journal of Veterinary Clinics
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    • v.20 no.3
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    • pp.369-375
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    • 2003
  • The ultrasonography was performed in 77,924 subestrous dairy cows from 680 dairy farms at 57 districts. The cows were examined for confirmation of resumption of ovaries and uterus after 30 days postpartum, for early pregnancy diagnosis after 30 days post-insemination, confirmation of pregnancy at 8 month post-insemination, and for diagnosis of reproductive dysfunctions, respectively. The results of reproductive examination by ultrasonography in 77,924 dairy cows were ovarian disorders 35,452 (46.8%), uterine disorders 10,721 (13.8%), pregnancy and pregnant failure 24,044 (30.8%), adhesion of reproductive tracts 167 (0.2%), freematins 13 (0.01%) and others 6,527 (8.4%) cows, respectively. The 13,732 (49.6%) cows out of 27,694 cows were treated for silent heat or error of estrus detection, 3,473 (12.5%) cows for follicular cysts, 815 (3.0%) cows for luteal cysts, 606 (2.2%) cows for inactive ovaries, 4 (0.01%) cows for granulosa cell tumors, and 6,455 (23.3%) cows for endometritis, respectively. The indices of reproductive efficiencies before (2001-08-10) and after (2003-07-20) periodical examination of reproductive status were as follows; the mean intercalving interval were shortened from 471 days to 383 days, the mean interval calving to conception were shortened from 187 days to 99 days, the mean interval calving to first service were shortened from 105 days to 67 days, the mean cows showing heat by 60 days postpartum were increased from 33% to 89%, the mean conception rate to first service were increased from 43% to 68%, and the mean service per conception were shortened from 2.6 times to 1.8 times, respectively. These results suggest that periodical examination of reproductive status would be useful for the improvement of the reproductive performance in dairy cows.

Progesterone assays as an aid for improving reproductive efficiency in dairy cattle V. Plasma progesterone determination as applied to the differential diagnosis of reproductive disorders and judgement of treatment responses to PGF2α or GnRH treatment (Progesterone 농도측정(濃度測定)에 의한 유우(乳牛)의 번식효율증진(繁殖效率增進)에 관한 연구(硏究) V. 혈장(血漿) progesterone 농도측정(濃度測定)에 의한 무발정(無發情)의 감별진단(鑑別診斷) 및 PGF2α 또는 GnRH 치료효과(治療效果)의 판정(判定))

  • Kang, Byong-kyu;Choi, Han-sun;Son, Chang-ho;Oh, Ki-seok;Kang, Hyun-ku;Kim, Sam-ju;Kim, Hyek-jin;Kim, Nam-ki
    • Korean Journal of Veterinary Research
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    • v.35 no.3
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    • pp.603-613
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    • 1995
  • Plasma progesterone($P_4$) assay has been introduced to apply to the differential diagnosis of reproductive disorders and the monitoring of responses of ovarian dysfunction to $PGF_2{\alpha}$ or GnRH treatment in the 204 postpartum and postinsemination subestrus dairy cows. 1. The incidence rate of reproductive disorders in 204 subestrus cows, diagnosed by palpation per rectum and plasma $P_4$ determination using 'Two sample test'(Day 0+Day 10) were as follows; silent heat or error of estrus detection 110(53.9%), persistent corpus luteum 26(12.7%), follicular cyst 16(7.8%), inactive ovary 12(5.9%), luteal cyst 11(5.4%), granulosa cell tumor of ovary 1(0.5%), fetal mummification 1(0.5%), endometritis 15(7.4%) and pyometra 12(5.9%), respectively. 2. After the $PGF_2{\alpha}$ treatment to the 76 cows with silent heat or error of estrus detection, persistent corpus luteum, or luteal cyst, plasma $P_4$ concentrations at day 3 post treatment using 'Two sample test'(Day 0+Day 3) remained low(<1.0ng/ml) in all 76 cows. Therefore all 76 cows responded positively to $PGF_2{\alpha}$ treatment. Seventeen cows with follicular cyst or inactive ovary were treated with GnRH. All 7 cows with follicular cyst and 4 cows with inactive ovary remained high($${\geq_-}1.0ng/ml$$) a plasma $P_4$ concentrations at day 12 post treatment using 'Two sample test'(Day 0+Day 12), but 6 cows with inactive ovary remained low(<1.0ng/ml) a plasma $P_4$ concentrations. Therefore all 7 cows with follicular cyst and 4 cows with inactive ovary responded positively, but 6 cows with inactive ovary responded negatively to GnRH treatment. 3. The mean days from treatment to first service, number of cows conceived on first service(%), mean number of services per conception, mean days from initial treatment to conception, and mean number of cows conceived by 100 days post treatment(%) were 5.0 and 26.2 days, 45(59.2%) and 6(35.3%) cows, 1.5 and 1.7 services, 13.6 and 22.6 days, and 62(81.6%) and 9(52.9%) cows in group of $PGF_2{\alpha}$ and GnRH treatment, respectively. These results indicated that plasma $P_4$ assay was practical as an aid to diagnosing reproductive disorders and to monitoring responses of ovarian dysfunction to $PGF_2{\alpha}$ and GnRH treatment in subestrus cows.

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Improvement of the Result Related to Tumor Marker Test Through the OCS QC Program (OCS QC 프로그램을 통한 건진 센터 종양검사의 결과보고 개선)

  • Back, Song-Ran;Kim, Sung-Ho;Yoo, So-Yeon;Kim, Nyun-Ok;Moon, Hyoung-Ho;Yoo, Seon-Hee;Cho, Shee-Man
    • The Korean Journal of Nuclear Medicine Technology
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    • v.13 no.3
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    • pp.185-188
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    • 2009
  • Purpose: Standard of retests were discrepant and inconsistent due to inaccuracy and lack of standardization within normal range limit of tumor marker test. To enhance the standardization of retests set standard value below normal range and the Order Communication System Quality Control (OCS QC) program was put in place. This program enables managing the results within lower limit of normal range which were used for tumor marker test in Health Center. Materials and Methods: At present the tumor marker study for AFP, CEA, CA19-9, CA125, and PSA included outpatients in Asan Medical Center from February to March, 2009. The standard value was obtained by using the percentage of CV of Inter Assay according to the normal range of each tumor test. The results were confirmed by using the OCS QC program via formatted assessment of screening test such as test items, standard value and medical department. The number of out-of-range results within plus and minus 30 percents regarding the five primary items of tumor marker test was assessed. The next step was to obtain the number of AFP, CEA, and CA125 according to the ratio of comparison between prior and post test result, 60%, 50%, and 40% within normal range, respectively. In addition, set standard value below normal range. Results: The first screening test with percentage of sample number was resulted between 30%-40% and the second one was AFP 26.1%, CEA 18.9%, CA19-9 17.3%, CA125 18.7%, and PSA 21.0% obtained screening percentage of average 20 percents. The limited value of retest was AFP less than 5.0 and more than 10.0, CEA less than 1.0 and more than 3.0, CA19-9 less than 10.0 and more than 30.0, and PSA less than 1.0 and more than 2.0 to set and the number of retest was obtained by applying to the limited value of retest to screening percentage of average 20 percents For two months, the number of retest was AFP 0, CEA 15, CA19-9 3, CA125 2, and PSA 5. Conclusions: Through using the OCS QC program in establishing the standard of retest systemically, there appeared to be reduced discrepancy among the examiners and to be expected improvement in relation to the error of results.

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