1 2 3 4 5 6 7 8 9 JAB RL358: -20082013 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 2 2013 8 XX 1 2008 2 1 29 30 31 32 33 2008-02-01-1/28-2 2013-07-XX
34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71...4...5...5...5...5...6 4.1...6 4.2...6 4.3...6 4.4...6 4.5...6 4.6...6 4.7...6 4.8...6 4.9...6 4.10...6 4.11...6 4.12...6 4.13...6 4.14...6 4.15...6...6 5.1...6 5.2...6 5.3...7 5.4...8 5.4.1...8 5.4.2...8 5.4.3...9 5.4.4...9 5.4.5...9 5.4.6... 10 5.4.7... 11 5.5... 11 5.6... 12 5.7... 15 2008-02-01-2/28-2 2013-07-XX
72 73 74 75 76 77 78 5.8... 15 5.9... 16 5.10... 18 A...19 B...22 C...24 2008-02-01-3/28-2 2013-07-XX
79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108 109 110 111 112 113 114 115 116 ( ) JAB JIS Q 17025:2005 (ISO/IEC 17025) JIS Q 17025 (ISO/IEC 17025):2005 JIS Q 17025 (ISO/IEC 17025):2005 JAB JAB RL355 () JAB RL359 ( ) JAB RL358 () (GMO)/ JIS Q 17025 (ISO/IEC 17025):2005 JIS Q 17025 (ISO/IEC 17025):2005 ISO 24276:2006 Foodstuffs Methods of analysis for the detection of genetically modified organisms and derived products General requirements and definitions CITAC/EURACHEM GUIDE, Guide to Quality in Analytical Chemistry, An Aid to Accreditation, Edition 2002 AOAC INTERNATIONAL Guidelines for Laboratories Performing Microbiological and Chemical Analyses of Food and Pharmaceuticals:2006 GUIDELINES ON PERFORMANCE CRITERIA AND VALIDATION OF METHODS FOR DETECTION, IDENTIFICATION AND QUANTIFICATION OF SPECIFIC DNA SEQUENCES AND SPECIFIC PROTEINS IN FOODS* CAC/GL 74-2010 ISO/TS 21098:2005 Foodstuffs Nucleic acid based methods of analysis of genetically modified organisms and derived products Information to be supplied and procedure for the addition of methods to ISO 21569, ISO 21570 or ISO 21571 5.10.9 JIS Q 17025(ISO/IEC 17025) JIS Q 17025:2005 JIS Q 17025 (ISO/IEC 17025):2005 JAB () 2008-02-01-4/28-2 2013-08-XX
117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 145 146 147 148 JAB ISO 24276:2006 Foodstuffs Methods of analysis for the detection of genetically modified organisms and derived products General requirements and definitions ISO/TS 21098:2005 Foodstuffs Nucleic acid based methods of analysis of genetically modified organisms and derived products Information to be supplied and procedure for the addition of methods to ISO 21569, ISO 21570 or ISO 21571 CAC/GL 74-2010 GUIDELINES ON PERFORMANCE CRITERIA AND VALIDATION OF METHODS FOR DETECTION, IDENTIFICATION AND QUANTIFICATION OF SPECIFIC DNA SEQUENCES AND SPECIFIC PROTEINS IN FOODS* CITAC/EURACHEM GUIDE Edition 2002 JAB CITAC Chairman JAB RL355 AOAC INTERNATIONAL Guidelines for Laboratories Performing Microbiological and Chemical Analyses of Food and Pharmaceuticals:2006 AOAC:2006JAB 2008-02-01-5/28-2 2013-08-XX
149 150 151 152 153 154 155 156 157 158 159 160 161 162 163 164 165 166 167 168 169 170 171 172 173 174 175 176 177 178 179 180 181 182 183 184 185 186 4.1 4.2 4.3 4.4 4.5 4.6 ISO 24276:2006 5.3.5 Material and reagents CITAC/EURACHEM GUIDE 14.2 - - 4.7 4.8 4.9 4.10 4.11 4.12 4.13 4.14 4.15 5.1 ISO 24276:2006 5 General Laboratory and procedural requirements 5.1 General 5.2 ISO 24276:2006 5.3.3 Personnel CITEC Guide 1 10 1 - CITAC/EURACHEM GUIDE 10.1-2 2008-02-01-6/28-2 2013-08-XX
187 188 189 190 191 192 193 194 195 196 197 198 199 200 201 202 203 204 205 206 207 208 209 210 211 212 213 214 215 216 217 218 219 220 221 222 223 224 225 226 5.2.2 CITAC/EURACHEM GUIDE 10.3 - - AOAC:2006 4.2.2-5.2.5 CITAC/EURACHEM GUIDE 10.4 - - i) ii) iii) OJT( ) iv) /() v) CITAC/EURACHEM GUIDE 10.5-5.3 ISO 24276:2006 5.3.2 Laboratory design ISO 24276:2006 5.3.3 Personnel 5.3.1 CITAC/EURACHEM GUIDE 12.4 - CITAC/EURACHEM GUIDE 12.6 2008-02-01-7/28-2 2013-08-XX
227 228 229 230 231 232 - CITAC/EURACHEM GUIDE 12.7-233 234 235 236 237 238 239 240 241 242 243 5.3.4 CITAC/EURACHEM GUIDE 12.3 - PCR i) ii) iii) iv) 244 245 246 247 248 249 5.4 5.4.1 CITAC/EURACHEM GUIDE 1.14.5-250 251 252 253 254 255 256 257 258 259 260 261 262 263 264 265 5.4.2 ISO 24276:2006 4.2 Guidance for the user on the selection of methods ISO 24276:2006 4.3 Performance characteristics ISO 24276:2006 5.2 Table 1 B CAC/GL 74-2010 ANNEX I PRACTICAL APPLICATION OF THE METHOD (27.~30.) CITAC/EURACHEM GUIDE 17.3 - ISO - ISO 21569:2005, Foodstuffs Methods of analysis for the detection of genetically modified organisms and derived products-qualitative nucleic acid based methods - ISO 21570:2005, Foodstuffs-Methods of analysis for the detection of genetically 2008-02-01-8/28-2 2013-08-XX
266 267 268 269 270 271 272 273 274 275 276 277 278 279 280 281 282 283 284 285 286 287 288 289 290 291 292 293 294 295 296 297 298 299 300 301 302 303 modified organisms and derived products-quantitative nucleic acid based methods - ISO 21571:2005, Foodstuffs-Methods of analysis for the detection of genetically modified organisms and derived products-nucleic acid extraction - ISO 21572:2004, Foodstuffs-Methods for the detection of genetically modified organisms and derived products-protein based methods - ISO/TS 21098:2005, Foodstuffs-Nucleic acid based methods of analysis of genetically modified organisms and derived products-information to be supplied and procedure for the addition of methods to ISO 21569, ISO 21570 or ISO 21571 5.4.3 5.4.4 5.4.5 5.4.5.1 ~ 5.4.5.3 ISO 24276:2006 6.6 ISO/TS 21098:2005 5 5.4.5.1 CAC/GL 74-2010 SECTION 1 INTRODUCTION (1. 2. 3.) CAC/GL 74-2010 SECTION 1.1 PURPOSE AND OBJECTIVES (4. 5.) CAC/GL 74-2010 SECTION 1.2 SCOPE (6.) 5.4.5.2 CAC/GL 74-2010 SECTION 2 METHOD VALIDATION (7.) CAC/GL 74-2010 Section 2.1 Criteria Approach (8.) CAC/GL 74-2010 Section 2.2 General Method Criteria (9.) CAC/GL 74-2010 Section 2.3 Validation Process (10. 11.) CAC/GL 74-2010 Section 3.1.6 Modular Approach to Method Validation (25. 26.) CAC/GL 74-2010 Section 3.2.1 General Information (27. 28. 29.) CAC/GL 74-2010 Section 3.2.2 Minimum Performance Requirements (30. 31. 32) CAC/GL 74-2010 Section 3.2.3 Collaborative Trial Test Materials (33. 34) CAC/GL 74-2010 ANNEX I DESCRIPTION OF THE METHOD (1.~5.) CAC/GL 74-2010 ANNEX I SPECIFIC INFORMATION REQUIRED FOR DNA-BASED METHODS (6.) CAC/GL 74-2010 ANNEX I Primer pairs (7.) CAC/GL 74-2010 ANNEX I Amplicon length(8) CAC/GL 74-2010 ANNEX I SPECIFIC INFORMATION REQUIRED FOR PROTEIN-BASED METHODS (14.~17.) CAC/GL 74-2010 ANNEX I INFORMATION ABOUT THE METHOD PERFORMANCE 2008-02-01-9/28-2 2013-08-XX
304 305 306 307 308 309 310 311 312 313 314 315 316 317 318 319 320 321 322 323 324 325 326 327 328 329 330 331 332 333 334 335 336 337 338 339 340 (18. 26.) CAC/GL 74-2010 ANNEX I PRACTICAL APPLICATION OF THE METHOD (27. 30.) 5.4.5.3 ISO 24276:2006 4.3 Performance characteristics CAC/GL 74-2010 Section 3.1 Method Development to Formal Validation (12) CAC/GL 74-2010 Section 3.1.1 Method Acceptance Criteria (Required condition for validation) CAC/GL 74-2010 Section 3.1.2 Applicability of the Method (15. 16.) CAC/GL 74-2010 Section 3.1.3 Principle condition (17. 18. 19. 20.) CAC/GL 74-2010 Section 3.2.4 Specific Information on the Validation of Methods (35. 36) 5.4.6 5.4.6.1 CAC/GL 74-2010 Section 3.1.5 Measurement Uncertainty (23. 24.) 5.4.6.1, 5.4.6.3 CITAC/EURACHEM GUIDE 16.3 - CITAC/EURACHEM GUIDE 16.5 - CITAC/EURACHEM GUIDE 16.8-10 CITAC/EURACHEM GUIDE 16.17-2008-02-01 -10/28-2 2013-08-XX
341 342 343 344 345 346 347 348 349 350 351 352 353 354 355 356 357 358 359 360 361 362 363 364 365 366 367 368 369 370 371 372 373 374 375 376 377 378 5.4.7 5.4.7.1, 5.4.7.2 CITAC/EURACHEM GUIDE 22.4 - - 5.5 5.5.1 CITAC/EURACHEM GUIDE 13.1.1 - i) ii) PCR iii) iv) 5.5.2 ISO 24276:2006 5.3.4 Apparatus and equipment CAC/GL 74-2010 ANNEX I whether the method is instrument or chemistry specific (9. 10. 11.) CITAC/EURACHEM GUIDE 11.12.3 - CITAC/EURACHEM GUIDE 13.3.5-2008-02-01 -11/28-2 2013-08-XX
379 380 381 382 383 384 385 386 387 388 389 390 391 392 393 394 395 396 397 398 399 400 401 402 403 404 405 406 407 408 409 410 411 412 413 414 415 416 5.5.6 CITAC/EURACHEM GUIDE 13.2.1 - CITAC/EURACHEM GUIDE 13.3.3 - A CITAC/EURACHEM GUIDE 13.3.4-5.5.9 CITAC/EURACHEM GUIDE 19.5-5.5.10 CITAC/EURACHEM GUIDE 19.5 - A 5.6 5.6.1 CITAC/EURACHEM GUIDE 19.5-5.6.2 5.6.2.2 5.6.2.2.1 CITAC/EURACHEM GUIDE 19.3.1 2008-02-01-12/28-2 2013-08-XX
417 418 419 420 421 422 423 424 425 426 427 428 429 430 431 432 433 434 435 436 437 438 439 440 441 442 443 444 445 446 447 448 449 450 451 452 453 454 - CITAC/EURACHEM GUIDE 19.3.2-5.6.2.2.2 CITAC/EURACHEM GUIDE 15.2 - ph CITAC/EURACHEM GUIDE 15.4 - CITAC/EURACHEM GUIDE 15.5 - SI SI CITAC/EURACHEM GUIDE 19.2-2 2008-02-01-13/28-2 2013-08-XX
455 456 457 458 459 460 461 462 463 464 465 466 467 468 469 470 471 472 473 474 475 476 477 478 479 480 481 482 483 484 485 486 487 488 489 490 491 492 (ISO 35:C6 ) CITAC/EURACHEM GUIDE 19.3.3 - CITAC/EURACHEM GUIDE 19.3.4-5.6.3 5.6.3.1 CITAC/EURACHEM GUIDE 20.6-3 1 5.6.3.2 CITAC/EURACHEM GUIDE 20.7 - CITAC/EURACHEM GUIDE 20.8-5.6.3.4 CITAC/EURACHEM GUIDE 20.9-2008-02-01 -14/28-2 2013-08-XX
493 494 495 496 497 498 499 500 501 502 503 504 505 506 507 508 509 510 511 512 513 514 515 516 517 518 519 520 521 522 523 524 525 526 527 528 529 530 CITAC/EURACHEM GUIDE 20.10-5.7 5.7.1 CITAC/EURACHEM GUIDE 11.5-1 CITAC/EURACHEM GUIDE 11.6 - CITAC/EURACHEM GUIDE 11.8-5.7.2 CITAC/EURACHEM GUIDE 11.14-5.7.3 CITAC/EURACHEM GUIDE 11.12.5-5.8 5.8.2 CITAC/EURACHEM GUIDE 11.15-2008-02-01 -15/28-2 2013-08-XX
531 532 533 534 535 536 537 538 539 540 541 542 543 544 545 546 547 548 549 550 551 552 553 554 555 556 557 558 559 560 561 562 563 564 565 566 567 568 JAB CITAC/EURACHEM GUIDE 12.1-5.8.3 CITAC/EURACHEM GUIDE 11.16-5.8.4 CITAC/EURACHEM GUIDE 11.13 - AOAC:2006 5.8.4-5.9 5.9.1 ISO/IEC 24276:2006 6.2 Interpretation of controls ISO/IEC 24276:2006 6.6 Quality assurance requirements CAC/GL 74-2010 Section 4 QUALITY CONTROL REQUIREMENTS (37. 38. 39. 40) CAC/GL 74-2010 ANNEX I SPECIFIC INFORMATION REQUIRED FOR PROTEIN-BASED METHODS (14.~17.) CAC/GL 74-2010 ANNEX I INFORMATION ABOUT THE METHOD PERFORMANCE (18. 26.) CAC/GL 74-2010 ANNEX I ANALYTICAL CONTROLS (31. 32.) CAC/GL 74-2010 ANNEX I METHOD PERFORMANCE (33.) 2008-02-01-16/28-2 2013-08-XX
569 570 571 572 573 574 575 576 577 578 579 580 581 582 583 584 585 586 587 588 589 590 591 592 593 594 595 596 597 598 599 600 601 602 603 604 605 606 5.9.1, 5.9.2 ISO/IEC 24276:2006 5.2 Use of controls CITAC/EURACHEM GUIDE 21.2 - QC CITAC/EURACHEM GUIDE 21.3 - QC QC QC CITAC/EURACHEM GUIDE 21.3.1 - QC QC CITAC/EURACHEM GUIDE 21.3.2 - QC QC QC QC QC CITAC/EURACHEM GUIDE 21.3.3-5 QC 20 QC QC 20% 50 QC CITAC/EURACHEM GUIDE 21.4 - QC 2008-02-01-17/28-2 2013-08-XX
607 608 609 610 611 612 613 614 615 616 617 618 619 620 621 622 623 624 625 626 627 628 629 630 631 632 633 634 635 636 C7 CITAC/EURACHEM GUIDE 21.5 - C7 ISO/IEC Guide43 B16 ILAC G13 5.10 5.10.1 ISO 24276:2006 6 Interpretation and expression of results 6.1 General ISO 24276:2006 6.3 Expression of a negative result ISO 24276:2006 6.4 Expression of a positive result ISO 24276:2006 6.5 Expression of ambiguous result CAC/GL 74-2010 Section 3.1.4 Unit of Measurement and reporting of results (21. 22) 5.10.2 ISO/IEC 24276:2006 7 Test report CITAC/EURACHEM GUIDE 11.12.7-5.10.3 ISO/IEC 24276:2006 7 Test report 2008-02-01-18/28-2 2013-08-XX
637 638 639 640 641 642 643 644 645 646 647 A A1. - - 5 1 3 1 1 1 5 1 1 2008-02-01-19/28-2 2013-08-XX
648 649 650 651 652 653 A2. - - (a) (b) (a) (b) (a) (b) (a) (b) (a) 2 (b) (a) 2 (b) (a) 2 (b) (a) 1 (b) ph 2 ( ) (a) (b) (b) 1 1 1 2008-02-01-20/28-2 2013-08-XX
PCR (a) (b) (a) (b) (a) (b) (c) / (a) (b) (c) ( ) 1 1 1 1 654 655 656 657 658 659 660 661 662 663 664 665 666 667 668 669 670 671 672 (accuracy) (trueness) (precision) ( JIS K 0211:2005 ) 2008-02-01-21/28-2 2013-08-XX
JAB RL358:2013 673 B ISO 24276:2006 Table-1 674 Control step b Environment Control Flow diagram showing intersection between successive steps and inclusion of controls c Extraction blank control d Positive extraction control DNA e Positive DNA target control DNA Negative DNA target control g Amplification reagent control PCR PCR inhibition control h Homogenization recommended Nucleic acid extraction a One per series Mandatory at regular intervals Assessment of nucleic acid quality Nucleic acid amplification Assessment of results of nucleic acid amplification Interpretation mandatory recommended mandatory i recommended, but mandatory in certain cases Test report :2008-02-01 22/28 2 2013-08-XX
JAB RL358:2013 a The arrows indicate that this control should be applied in the subsequent analytical steps. b The use of environment controls will help the laboratory to identify sources of contamination at an early stage and can even be used to identify in which work area the contamination is present. c DNA 8 96 1 At least one extraction blank control shall be included each time DNA is extracted from one or more samples. The tube shall always be the last in each series. It may be appropriate to put one extraction blank on e. g. a rack of eight tubes or a microplate of 96 wells for automated extraction. d A positive extraction control should be included regularly, and always when a new batch of extraction reagents is used. This control will reveal if something is wrong with the reagents or the performance of the extraction of the extraction protocol. e DNA GMO target taxon The positive DNA target control demonstrates the ability of the nucleic acid amplification procedure to detect the nucleic acid representative of the GMO or target taxon. This condition can also be fulfilled by an appropriate positive extraction control. f DNA GMO target taxon The negative DNA target control demonstrates the ability of the nucleic acid amplification procedure to avoid false positive amplification in the absence of the nucleic acid representative of the GMO or target taxon. g PCR The amplification reagent control demonstrates the absence of contaminating nucleic acid in the PCR reagent batches used. The amplification reagent control can be omitted when the extraction blank control is used. h PCR The PCR inhibition control may be used to demonstrate the absence of soluble inhibitors. This may also be demonstrated by serial dilutions of the template nucleic acid. However, some type of assessment of the effect of soluble inhibitors on the results of the analysis of the sample shall be made. i PCR DNA PCR A PCR-inhibition control is mandatory, if all PCR-tests on the sample are negative and for matrices where the yield of amplifiable DNA is not known. :2008-02-01 23/28 2 2013-08-XX
JAB RL358:2013 675 676 677 678 679 680 681 682 683 684 685 686 687 688 689 690 691 692 693 694 695 696 697 698 699 700 701 702 703 704 705 706 707 708 709 710 C ISO 24276:2006 6.2 Interpretation of controls Each control has a valid value and, if the observed result for any control is different from the valid value, the analysis shall be repeated. Environmental controls may be positive (amplification product of expected size detected) or negative (no amplification product detectable), but a positive result shall always initiate measures to remove and prevent contamination of the laboratory environment. If a non-valid result for any of the other controls is obtained repeatedly, measures shall be taken to locate and remove/replace the source(s) responsible for the error, and the analysis then repeated. Analytical results shall only be reported when all controls yield valid values. The valid values for the controls are as follows: - positive extraction controls shall always be positive; - - extraction blank controls shall always be negative; - DNA positive DNA target controls shall always be positive; - DNA negative DNA target controls shall always be negative; - amplification reagent controls shall always be negative. PCR ( :2008-02-01 24/28 2 2013-08-XX
JAB RL358:2013 711 712 713 714 715 716 717 718 719 ) PCR-inhibition controls shall not show significant inhibitory effects on the reaction (for qualitative analysis, the effect of inhibition may be less important than for quantitative analysis). PCR Possible PCR results of the controls are listed in Table 2. These are used for interpreting/reporting the test sample result. :2008-02-01 25/28 2 2013-08-XX
JAB RL358:2013 720 721 PCR Test sample Positive extraction control Extraction blank control DNA Negative DNA target control DNA Positive DNA target control + a + - - b + - + - - + + + + - + - - + - - - - - - - a PCR PCR product is detectable. Interpreted result positive negative c inconclusive c inconclusive d inconclusive b PCR No PCR product is detectable. c The procedure is repeated beginning with the extraction step (possible contamination). 722 d The procedure is repeated using another extraction method or a further purification step (possible inhibition). :2008-02-01 26/28 2 2013-08-XX
JAB RL358:2013 723 724 725 726 JAB NF18 REV.0 1 2008-02-01 JIS Q 17025 2013-07-XX PM () 727 728 729 730 731 732 733 :2008-02-01 27/28 2 2013-08-XX
JAB RL358:2013 734 735 736 737 738 739 740 741 742 743 744 745 746 747 748 749 750 751 752 753 754 755 756 757 758 759 760 761 762 763 141-0022 1 22-1 AN 3F Tel.03-3442-1217 Fax.03-5475-2780 :2008-02-01 28/28 2 2013-08-XX