KS Q ISO 11843-5-2012 Capability of detection－Part 5：Methodology in the linear and non-linear calibration cases《检测能力 第5部分 线性和非线性校准容器中的方法学》.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS Q ISO 11843 5 5： KS Q ISO 11843 5:2012 2012 8 22 http： /www.kats.go.krKS Q ISO 11843 5:2012 ： ( ) ( ) ( ) ： (http：/www.standard.go.kr) ： ：2012 8 22 2012-0380 ： ： ( 02-509-7274) (http：/www.kats.go.kr). 10 5 , . KS Q ISO 11843 5:2012 i ii 1 .1 2 2 3 .2 4 4

2、5 5 5.1 .5 5.2 .6 5.3 .6 5.4 .6 6 7 6.1 .7 6.2 .7 6.3 9 6.4 ELISA 9 A( ) 11 B( ) (9) 12 C( ) (13) 13 14 KS Q ISO 11843 5:2012 ii 2008 1 ISO 11843 5, Capability of detection Part 5： Methodology in the linear and non-linear calibration cases . KS Q ISO 11843 5:2012 5： Capability of detection Part 5： M

3、ethodology in the linear and non-linear calibration cases 1 . . , (SD) (CV) . KS Q ISO 11843 2 . , , (POP) (ELISA) , . KS Q ISO 11843 1 KS Q ISO 11843 2 . KS Q ISO 11843 2 . xc xd . xc xd , . xc xd . , , . / . SD CV . . KS Q ISO 11843 5:2012 2 2 . . ( ) . KS A ISO 5725 1, ( ) 1： KS Q ISO 3534 1, 1：

4、KS Q ISO 3534 2, 2： KS Q ISO 3534 3, 3： KS Q ISO 11843 1, 1： KS Q ISO 11843 2, 2： 3 KS Q ISO 3534( ), KS A ISO 5725 1, KS Q ISO 11843 1, KS Q ISO 11843 2 . 3.1 (critical value of the net state variable) xc X KS Q ISO 11843 1： 2009, 2.10 1 . 3.2 (minimum detectable value of the net state variable) xd

5、 1 ISO 11843 1： 1997, 11. ISO 11843 1： 1997/Cor.1： 2003 . 1 . 3.3 (precision) (SD) SD 1 SD (CV) . 2 (KS Q ISO 3534 2) . 3 , , , . KS Q ISO 11843 5:2012 3 xc xd X X 0 1 X xd 2 a KS Q ISO 11843 1： 2009 1 . 1 KS Q ISO 11843 1 . 1 X 0( ) xd ( ) 3.4 (precision profile) . 3.5 (response variable) Y KS Q IS

6、O 3534 3： 2009, 1.2 1 ISO 11843 . Z . 2 Y , KS Q ISO 11843 5:2012 4 , X(X) X(X) . 3.6 (precision profile of response variable) (pipetting), 3.7 (net state variable) X Z z0 KS Q ISO 11843 1： 2009, 4. X , X(X) X(X) . 4 , (SD CV) Y( X ) . , Y X , 21,2 . 2 3 , SD, Y(X) |dY / dX| SD, X(X) . X CV X(X) . X

7、YXYXXYXdd)()( = (1) Y(X) X , X(X) (1) X . |dY / dX| . 1 (Y aX) , X(X) Y(X) . Y aX Y/X |dY/dX|=a . 2 X 0 (1) , SD, X(X) (= Y(X)Y/|dY / dX|) X X(X) . KS Q ISO 11843 5:2012 5 3 |dY / dX| SD, Y SD, X 5 5.1 . xc . xc kcX(0) (2) kc ： X(0) ： X 0 SD X(0) Y(0)/ |dY/dX | , (2) xc kcY(0)/ |dY/dX | . xd . xd xc

8、 kdX(xd) (3) kd ： X(xd) ： X xd( 1 ) SD KS Q ISO 11843 5:2012 6 X(X)(3.4 ) xc xd . 1 kc kd 1.65 = = 5 % . 2 X(X) X(X) X kc kd 1.65 , (2) (3) xc 1.65X xd 3.30X . 5.2 X(xd) SD X 0 X(0) xc xd . xc kcX(0) (4) xd (kc kd)X(0) (5) (4) (2) , . . X(X) . X(X) X(X) X kc kd 1.65 , (4) (5) xc 1.65X xd 3.30X . 5.3

9、 5.2 X(0) X(xd) , xc xd . xc kcX(xd) (6) xd (kc kd)X(xd) (7) , . X(X) X(X) X kc kd 1.65 , (6) (7) xc 1.65X xd 3.30X . 5.4 5.3 (10) . (7) . X(xd) X(xd)/xd 1/(kc kd)(8) X xd CV . (8) xd CV 1/(kc kd)100 % . xc xd X(X) . (Y lg X) dY/dlg X X , . )()2.303(dlgdddcdxkkXYYxX+=(9) X xd(ln 10 2.303) |dY /dlg X

10、| . , ( ) . (9) B . 1 kc kd 1.65 , (8) X(X) 1/3.30 30 % . xd X CV KS Q ISO 11843 5:2012 7 30 % . 2 kc kd 1.65 , (9) . 132.0)(dlgdddxXYYxX= (10) , 0.132 1/(3.32.303) . 6 6.1 6.2 6.3 SD CV (3.4 ) . X(X) 4. SD CV . 6.4 ELISA . 6.4 ELISA , . 6.2 17- ELISA . 4 . 96 (well) . , . . ELISA . Y( ) ( ) 1. BGXG

11、Y+ X： ( ) G ： B ： 3 , Y CV, Y(X)2 1. ()222)( +=YrrrrG(XXXW2S2B2X2G2Y (11) , X ： ( ) Y ： ( ). G ： (0.1 g/L) rX： CV(0.9 %) rG： CV(0.9 %) rB： CV(1.9 %) rS： (2/3)( CV). 2/3 KS Q ISO 11843 5:2012 8 (0.6 %) . W： SD. (0.002 ) X(X) 2 (11) . 4 ELISA X(X) 5 . CV, X(X) (11) , . 5.3 xd ( 5 ). 30 % CV 5.4 1 . 50

12、 L 50 L 50 L 100 L 30 100 L KS Q ISO 11843 5:2012 9 . 5 b) X 0 CV . . CV . a) b) 5 17- ELISA CV, X(X) ( ) xd 6.3 , 2. Y(X)2 Yj (12) , Y(X) Y SD . j 0 . j 1 . j 2 , CV, Y(X) . . 6.4 ELISA 0.02 0.04 0.06 0.08 0.1 0.001 0.01 0.1 1 10 100 KS Q ISO 11843 5:2012 10 ELISA B/B0 , (10) 4. 132.0)(dlgddd1xX/CX

13、11YxXC2=+= (13) , Y(xd) xd CV . C . (13) . 6 17- ELISA( 6.2 ) B/B0 . 1.9 % CV CV Y(xd) (13) 0.15( 0.019 / 0.132) . xd ( 6 ). 1： (13) . 2： 1 B/B0 . 3： X . X xd . 6.2 ( 5 6 ). 1, 2, 3 6.4 1, 2, 3 6 17- ELISA B/B0 0.001 0.01 0.1 1 10 100 KS Q ISO 11843 5:2012 11 A ( ) SD (standard deviation) CV (SD )co

14、efficient of variation (SD divided by the mean) POP (persistent organic pollutant) ELISA (enzyme-linked immunosorbent assay) X (net state variable) Y (response variable) xc (critical value of net state variable) xd (minimum detectable value of net state variable) kc (coefficient to specify ) kd (coe

15、fficient to specify ) X 0 1 (probability of an error of the first kind at X 0) X xd 2 (probability of an error of the second kind at X xd) Y(X) X SD(SD of response variable as a function of X) Y(X) X CV(CV of response variable as a function of X) X(X) X SD(SD of net state variable as a function of X

16、) X(X) X CV(CV of net state variable as a function of X) |dY / dX | (derivative of calibration function) B/B0 0 (ratio of measurements for arbitrary dose to measurements for zero dose) KS Q ISO 11843 5:2012 12 B ( ) (9) (1) xd (7) . XYXXYXdd)()( = ddddcddddcdddcddlnd)()(1dlnd)()(dd)()(xXYxXYxXYXYxxk

17、kxXYxkkXYxkkx=+=+=+= , . xd . )()(dlndddcdxkkXYYxX+= (In X 2.303 lg X) (9) . 4 . KS Q ISO 11843 5:2012 13 C ( ) (13) ELISA 4 . 312301CCXCCYC+= B/B0 . 12011CCXBB+= C0, C1, C2, C3 . dY (C0 C3)dB/B0 (10) , 0.132)/(dlgd0 3Y0CCXXB/B = C0 (X 0) C3 (X ) , Y(X)/(C0 C3) Y(X)/C0 . Y(X) , 030)()()(CXCCXXYYY =

18、Y(X)/C0 , Y(0) CV . (13) . 4 . KS Q ISO 11843 5:2012 14 1 Hayashi, Y., Matsuda, R., Maitani, T., Imai, K., Nishimura, W., Ito, K. and Maeda, M. Precision, limit of detection and range of quantitation in competitive ELISA. Anal. Chem., 76(5), 2004, pp. 1 2951 301 2 Dudley, R.A., Edwards, P., Ekins, R

19、.P., Finney, D.J., McKenzie, I.G.M., Raab, G.M., Rodbard, D. and Rodgers, R.P.C. Guidelines for immunoassay data processing. Clin. Chem., 31(8), 1985, pp. 1 2641 271 3 Guide to the expression of uncertainty in measurement (GUM), BIPM, IEC, IFCC, ISO, IUPAC, IUPAP, OIML, 19931)4 Hayashi, Y., Matsuda,

20、 R., Ito, K., Nishimura, W., Imai, K. and Maeda, M. Detection limit estimated from slope of calibration curve： An application to competitive Elisa. Anal. Sci., 21, 2005, pp. 167169 5 KS Q ISO 3534 3： 2009, 3： 1) 1995 . 5： 153787 1 92 3(13) (02)26240114 (02)262401489 http：/ Korean Agency for Technology and Standards http： /www.kats.go.kr KS Q ISO 11843 5:2012 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Capability of detection Part 5：Methodology in the linear and non-linear calibration cases ICS 03.120.30 ; 17.020