• Title/Summary/Keyword: Dilution of Precision

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A comparison study of 76Se, 77Se and 78Se isotope spikes in isotope dilution method for Se (셀레늄의 동위원소 희석분석법에서 첨가 스파이크 동위원소 76Se, 77Se 및 78Se들의 비교분석)

  • Kim, Leewon;Lee, Seoyoung;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.170-178
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    • 2016
  • Accuracy and precision of ID methods for different spike isotopes of 76Se, 77Se, and 78Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and 78Se showed was a bit better than 76Se and 77Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for 78Se, 76Se and 77Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of 78Se isotope spike (over 100 % RSD). 76Se and 77Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, 78Se should be avoided when large amount of Br exists in matrix. Either 76Se or 77Se would provide accurate results.

Determination of plasma C16-C24 globotriaosylceramide (Gb3) isoforms by tandem mass spectrometry for diagnosis of Fabry disease (패브리병(Fabry) 진단을 위한 혈장 중 Globotriaosylceramide (Gb3)의 탠덤매스 분석법 개발과 임상 응용)

  • Yoon, Hye-Ran;Cho, Kyung-Hee;Yoo, Han-Wook;Choi, Jin-Ho;Lee, Dong-Hwan;Zhang, Kate;Keutzer, Joan
    • Journal of Genetic Medicine
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    • v.4 no.1
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    • pp.45-52
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    • 2007
  • Purpose : A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-ex tensive pre-treatment by electrospray ionization MS/ MS (ESI-MS/MS). Measurement of globotriaosy lceramide (Gb3, ceramide trihex oside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. Methods : Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Results : Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms w as found in the range of 0.001-1.0 ${\mu}g$/mL. The limit of detection (S/N=3) was 0.001 ${\mu}g$/mL and limit of quantification was 0.01 ${\mu}g$/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. Conclusion : This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

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Improvement of GPS positioning accuracy by static post-processing method (정적 후처리방식에 의한 GPS의 측위정도 개선)

  • 김민선;신현옥
    • Journal of the Korean Society of Fisheries and Ocean Technology
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    • v.39 no.4
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    • pp.251-261
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    • 2003
  • To measure the GPS position accuracy and its distribution according to the length of the baseline, 30 minutes to 24 hours observations at the fixed location were conducted with two GPS receivers (Ll, 12 channels) on May 29 to June 2, 2002. The GPS data received at the reference station, the rover station and the ordinary times GPS observation station operated by the National Geography Institute in Korea were processed in kinematic and static post-processing methods with a post -processing software. The results obtained are summarized as follows: 1. The number of the satellite that could be observed continuously more than six hours was 16 and most of these satellites were positioned at east-west direction on May 31, 2002. The number of the satellite observed and the geometric dilution of precision (GDOP) determined by the average of every 10 minute for the day were 8 and 3.89, respectively. 2. Both the average GPS positions before and after post-processing were shifted (standalone: 1.17 m, post -processing: 0.43m) to the south and west. The twice distance root mean square (2drms) measured with standalone was 6.65m. The 2drms could be reduced to 33.8% (standard deviation 0=17.2) and 5.3% (0=2.2) of standalone by the kinematic and the static post-processing methods, respectively. 3. The relationship between the length of the baseline x (km) and the 2drms y (m) obtained by the static post-processing method was y=0.00l6x+0.006 $(R^2=0.87)$. In the case of the positioning with the static post-processing method using the GPS receiver, it was found that a positioning within 20cm 2drms was possible when the length of the baseline was less than 100km and the receiving time of the GPS is more than 30 minutes.