Standard Test Method for Determination of Cannabinoid Concentration in Dried Cannabis and Hemp Raw Materials using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

Importancia y uso:

5.1 The analysis and reporting of cannabinoid content in cannabis and hemp is required to address human health and safety concerns, satisfy testing and labeling requirements, and meet the regulatory guidelines of various jurisdictions. This test method is useful in providing quantitative results for up to seventeen cannabinoids in dried cannabis and hemp raw material samples.

Subcomité:

D37.03

Referida por:

D8442-22

Volúmen:

15.10

Número ICS:

11.120.99 (Other standards related to pharmaceutics)

Palabras clave:

analyses; cannabinoids; cannabis; hemp; laboratory; LC-MS/MS Δ9-THC Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.318 48.9 (%) (%) Batch-1 n 6 6 6 6 6 6 - - - Av. 8.41 27.8 1474 7428 0.279 50.3 - - Precision (%) 0.7 % 1.5 % 0.8 % 0.2 % 0.5 % 0.9 % - - Accuracy (%) 84.1 % 92.5 % 98.3 % 92.8 % 87.8 % 103.0 % - - Batch-2 n 6 6 6 6 6 6 - - - Av. 9.17 29.2 1529 7644 0.278 46.0 - - Precision (%) 1.0 % 1.3 % 0.6 % 0.8 % 0.8 % % - - Accuracy (%) 91.7 % 97.5 % 101.9 % 95.6 % 87.3 % 94.0 % - - Batch-3 n 6 6 6 6 6 6 1 - Av. 9.00 27.6 1503 7368 0.275 46.3 - - Precision (%) 1.1 % 0.6 % 0.5 % 0.3 % 0.9 % 0.7 % - - Accuracy (%) 90.0 % 92.1 % 100.2 % 92.1 % 86.4 % 94.8 % 95.6 % - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 8.86 28.2 1502 7480 0.28 47.6 - - Precision (%) 3.9 % 2.9 % 1.6 % 1.7 % 1.0 % 5.0 % - - Accuracy (%) 88.6 % 94.0 % 100.1 % 93.5 % 87.2 % 97.3 % - - Δ9-THCA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.979 124 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.83 28.1 1467 7437 1.01 119 - - Precision (%) 2.2 % 1.3 % 0.3 % 0.8 % 1.0 % 1.2 % - - Accuracy (%) 88.3 % 93.6 % 97.8 % 93.0 % 102.8 % 95.9 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.07 29.1 1507 7564 0.961 106 - - Precision (%) 1.0 % 0.9 % 0.4 % 1.0 % 1.2 % 3.0 % - - Accuracy (%) 90.7 % 97.0 % 100.5 % 94.6 % 98.1 % 85.3 % - - Batch-3 n 6 6 6 6 6 6 - - Av. 9.1 27.3 1520 7358 0.970 111 - - Precision (%) 2.2 % 1.7 % 0.6 % 0.8 % 1.4 % 0.4 % - - Accuracy (%) 91.3 % 91.0 % 101.3 % 92.0 % 99.1 % 89.5 % - - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.01 28.2 1498 7453 0.979 112 - - Precision (%) 2.3 % 3.0 % 1.6 % 1.4 % 2.4 % 5.3 % - - Accuracy (%) 90.1 % 93.8 % 99.9 % 93.2 % 100.0 % 90.2 % - - CBD Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 5.41 8.33 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.9 27.8 1465 7634 5.15 8.60 - - Precision (%) 3.1 % 2.3 % 0.5 % 1.2 % 1.2 % 1.9 % - - Accuracy (%) 88.6 % 92.7 % 97.7 % 95.4 % 95.3 % 103.2 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.4 28.8 1491 7651 5.07 7.59 - - Precision (%) 5.1 % 1.2 % 0.6 % 1.0 % 1.5 % 3.8 % - - Accuracy (%) 94.2 % 96.0 % 99.4 % 95.6 % 93.7 % 91.2 % - - Batch-3 n 6 6 6 6 6 6 - - Av. 9.2 27.5 1494 7483 5.04 7.97 - - Precision (%) 4.6 % 1.1 % 0.9 % 1.5 % 1.1 % 2.1 % - - Accuracy (%) 92.5 % 91.8 % 99.6 % 93.5 % 93.2 % 95.7 % - - QC sample Inter-Batch Stats n 18 18 18 18 18 18 Av. 9.18 28.1 1483 7589 5.09 8.06 - - Precision (%) 4.9 % 2.5 % 1.1 % 1.6 % 1.5 % 5.9 % - - Accuracy (%) 91.8 % 93.5 % 98.9 % 94.9 % 94.0 % 96.7 % - - CBDA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 14.6 23.0 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 9.1 27.6 1462 7584 13.5 23.5 - - Precision (%) 3.1 % 2.8 % 1.4 % 1.7 % 2.0 % 1.8 % - - Accuracy (%) 90.8 % 91.9 % 97.4 % 94.8 % 92.3 % 102.1 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.2 28.7 1500 7684 13.4 20.2 - - Precision (%) 2.9 % 2.2 % 0.9 % 1.0 % 1.7 % 4.0 % - - Accuracy (%) 92.1 % 95.6 % 100.0 % 96.1 % 91.5 % 87.7 % - - Batch-3 n 6 6 6 6 6 6 - - Av. 9.2 27.7 1529 7420 13.4 22.2 - - Precision (%) 2.5 % 2.8 % 0.7 % 1.4 % 2.2 % 1.6 % - - Accuracy (%) 91.8 % 92.4 % 101.9 % 92.8 % 92.0 % 96.4 % - - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.16 28.0 1497 7563 13.4 21.9 - - Precision (%) 2.7 % 3.1 % 2.1 % 2.0 % 1.9 % 6.8 % - - Accuracy (%) 91.6 % 93.3 % 99.8 % 94.5 % 91.9 % 95.4 % - - CBG Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.048 2.14 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 9.0 27.6 1431 7572 0.0383 1.70 - - Precision (%) 2.0 % 1.2 % 0.8 % 0.5 % 2.9 % 0.8 % - - Accuracy (%) 90.5 % 92.1 % 95.4 % 94.6 % 80.1 % 95.5 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.5 28.7 1481 7763 0.0382 1.59 - - Precision (%) 1.6 % 1.4 % 1.2 % 1.1 % 1.9 % 1.9 % - - Accuracy (%) 95.4 % 95.7 % 98.7 % 97.0 % 80.0 % 89.6 % - - Batch-3 n 6 6 6 6 6 6 1 - Av. 9.0 26.8 1498 7562 0.0383 1.60 - - Precision (%) 2.2 % 1.5 % 1.1 % 0.7 % 1.2 % 1.8 % - - Accuracy (%) 89.7 % 89.4 % 99.8 % 94.5 % 80.2 % 90.0 % 102.1 - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.18 27.7 1470 7632 0.038 1.63 - - Precision (%) 3.4 % 3.1 % 2.2 % 1.5 % 2.0 % 3.3 % - - Accuracy (%) 91.8 % 92.4 % 98.0 % 95.4 % 80.1 % 91.7 % - - CBGA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.117 3.89 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.5 27.9 1464 7392 0.110 3.97 - - Precision (%) 0.9 % 1.0 % 0.7 % 0.9 % 1.5 % 1.0 % - - Accuracy (%) 84.9 % 92.9 % 97.6 % 92.4 % 93.9 % 102.1 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.3 29.2 1509 7487 0.106 3.53 - - Precision (%) 2.1 % 1.1 % 0.6 % 0.8 % 1.5 % 3.3 % - - Accuracy (%) 93.2 % 97.4 % 100.6 % 93.6 % 90.7 % 90.6 % - - Batch-3 n 6 6 6 6 6 6 1 - Av. 8.9 27.6 1518 7426 0.107 3.76 - - Precision (%) 2.5 % 1.4 % 0.4 % 0.6 % 0.9 % 0.7 % - - Accuracy (%) 89.4 % 91.9 % 101.2 % 92.8 % 91.6 % 96.5 % 103.5 - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 8.91 28.2 1497 7435 0.108 3.75 - - Precision (%) 4.3 % 2.9 % 1.7 % 0.9 % 2.0 % 5.3 % - - Accuracy (%) 89.1 % 94.1 % 99.8 % 92.9 % 92.1 % 96.4 % - - CBGV Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 - - (%) (%) Batch-1 n 6 6 6 6 - - - - Av. 9.0 27.5 1417 7617 - - - - Precision (%) 3.9 % 1.8 % 0.8 % 0.7 % - - - - Accuracy (%) 89.9 % 91.5 % 94.5 % 95.2 % - - - - Batch-2 n 6 6 6 6 - - - - Av. 9.7 28.4 1472 7775 - - - - Precision (%) 1.7 % 1.4 % 1.1 % 0.9 % - - - - Accuracy (%) 97.1 % 94.6 % 98.1 % 97.2 % - - - - Batch-3 n 6 6 6 6 - - 1 1 Av. 9.2 26.7 1474 7643 - - - - Precision (%) 3.7 % 1.8 % 1.2 % 0.8 % - - - - Accuracy (%) 92.4 % 89.2 % 98.3 % 95.5 % - - 98.4 97.0 QC sample Inter-Batch Stats n 18 18 18 18 - - - - Av. 9.32 27.5 1454 7678 - - - - Precision (%) 4.5 % 3.0 % 2.1 % 1.2 % - - - - Accuracy (%) 93.2 % 91.8 % 97.0 % 96.0 % - - - - CBGVA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 - - (%) (%) Batch-1 n 6 6 6 6 - - - - Av. 8.5 28.9 1497 7238 - - - - Precision (%) 3.1 % 0.9 % 1.2 % 1.3 % - - - - Accuracy (%) 85.5 % 96.2 % 99.8 % 90.5 % - - - - Batch-2 n 6 6 6 6 - - - - Av. 9.2 30.3 1563 7395 - - - - Precision (%) 1.9 % 2.0 % 0.9 % 1.1 % - - - - Accuracy (%) 92.0 % 101.0 % 104.2 % 92.4 % - - - - Batch-3 n 6 6 6 6 - - 1 1 Av. 8.9 28.7 1562 7203 - - - - Precision (%) 1.9 % 0.6 % 0.5 % 0.7 % - - - - Accuracy (%) 88.8 % 95.7 % 104.1 % 90.0 % - - 102.5 102.5 QC sample Inter-Batch Stats n 18 18 18 18 - - - - Av. 8.88 29.3 1541 7278 - - - - Precision (%) 3.8 % 2.8 % 2.2 % 1.5 % - - - - Accuracy (%) 88.8 % 97.7 % 102.7 % 91.0 % - - - - CBN Precision, Accuracy and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.490 3.39 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.9 27.1 1426 7575 0.461 3.70 - - Precision (%) 2.3 % 2.0 % 0.7 % 0.6 % 1.1 % 0.9 % - - Accuracy (%) 88.6 % 90.5 % 95.1 % 94.7 % 94.0 % 109.2 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.6 28.7 1487 7767 0.453 3.41 - - Precision (%) 1.4 % 1.0 % 0.3 % 0.8 % 1.7 % 4.7 % - - Accuracy (%) 95.8 % 95.5 % 99.1 % 97.1 % 92.5 % 100.6 % - - Batch-3 n 6 6 6 6 6 6 1 - Av. 9.3 27.4 1489 7533 0.459 3.30 - - Precision (%) 1.5 % 0.9 % 0.5 % 0.3 % 1.0 % 0.4 % - - Accuracy (%) 93.4 % 91.5 % 99.3 % 94.2 % 93.6 % 97.4 % 96.2 - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.26 27.7 1467 7625 0.458 3.47 - - Precision (%) 3.7 % 2.7 % 2.1 % 1.5 % 1.4 % 5.6 % - - Accuracy (%) 92.6 % 92.5 % 97.8 % 95.3 % 93.4 % 102.4 % - - CBNA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.350 1.84 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.7 28.7 1488 7471 0.365 2.11 - - Precision (%) 4.4 % 2.5 % 0.8 % 1.2 % 1.8 % 3.1 % - - Accuracy (%) 87.4 % 95.6 % 99.2 % 93.4 % 104.2 % 114.4 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 8.7 29.1 1510 7565 0.337 1.86 - - Precision (%) 4.9 % 2.7 % 1.4 % 0.8 % 2.6 % 4.5 % - - Accuracy (%) 87.4 % 97.1 % 100.7 % 94.6 % 96.2 % 101.3 % - - Batch-3 n 6 6 6 6 6 6 1 - Av. 9.0 28.3 1513 7332 0.340 1.88 - - Precision (%) 3.6 % 3.3 % 0.9 % 1.4 % 1.8 % 2.0 % - - Accuracy (%) 90.2 % 94.3 % 100.9 % 91.7 % 97.3 % 101.9 % 103.8 - QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 8.83 28.7 1504 7456 0.347 1.95 - - Precision (%) 4.3 % 2.9 % 1.3 % 1.7 % 4.1 % 6.7 % - - Accuracy (%) 88.3 % 95.7 % 100.2 % 93.2 % 99.2 % 105.9 % - - CBV Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 - - (%) (%) Batch-1 n 6 6 6 6 - - - - Av. 8.6 27.0 1447 7629 - - - - Precision (%) 2.7 % 1.0 % 1.1 % 0.5 % - - - - Accuracy (%) 85.7 % 90.1 % 96.5 % 95.4 % - - - - Batch-2 n 6 6 6 6 - - - - Av. 9.6 28.8 1472 7755 - - - - Precision (%) 4.8 % 2.4 % 1.6 % 1.3 % - - - - Accuracy (%) 96.3 % 96.0 % 98.1 % 96.9 % - - - - Batch-3 n 6 6 6 6 - - 1 1 Av. 9.2 27.1 1483 7395 - - - - Precision (%) 3.8 % 1.4 % 1.5 % 1.0 % - - - - Accuracy (%) 92.0 % 90.5 % 98.9 % 92.4 % - - 100.7 99.9 QC sample Inter-Batch Stats n 18 18 18 18 - - - - Av. 9.13 27.7 1467 7593 - - - - Precision (%) 6.1 % 3.4 % 1.7 % 2.2 % - - - - Accuracy (%) 91.3 % 92.2 % 97.8 % 94.9 % - - - - CBC Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.325 1.18 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 9.0 27.1 1413 7756 0.276 1.03 - - Precision (%) 3.4 % 2.1 % 0.9 % 0.6 % 1.6 % 3.0 % - - Accuracy (%) 89.6 % 90.3 % 94.2 % 97.0 % 85.1 % 100.7 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.3 28.9 1457 7878 0.268 1.04 - - Precision (%) 3.4 % 1.7 % 0.9 % 1.1 % 0.8 % 1.9 % - - Accuracy (%) 92.7 % 96.5 % 97.1 % 98.5 % 82.5 % 101.9 % - - Batch-3 n 6 6 6 6 6 6 1 1 Av. 9.6 27.3 1435 7630 0.268 1.03 - - Precision (%) 4.2 % 1.9 % 0.7 % 0.5 % 1.4 % 1.1 % - - Accuracy (%) 96.2 % 91.1 % 95.7 % 95.4 % 82.5 % 101.4 % 93.0 89.4 QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.29 27.8 1435 7755 0.271 1.03 - - Precision (%) 4.6 % 3.5 % 1.5 % 1.5 % 1.9 % 2.0 % - - Accuracy (%) 92.9 % 92.6 % 95.7 % 96.9 % 83.4 % 101.3 % - - CBCA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.448 1.67 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.9 27.8 1448 7612 0.400 1.70 - - Precision (%) 4.1 % 3.5 % 2.0 % 0.8 % 1.4 % 2.7 % - - Accuracy (%) 89.5 % 92.5 % 96.5 % 95.1 % 89.4 % 101.6 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.7 29.4 1468 7756 0.389 1.54 - - Precision (%) 2.6 % 2.3 % 1.0 % 1.7 % 1.6 % 1.9 % - - Accuracy (%) 97.3 % 98.1 % 97.9 % 96.9 % 86.8 % 91.9 % - - Batch-3 n 6 6 6 6 6 6 1 1 Av. 9.1 27.3 1479 7601 0.385 1.60 - - Precision (%) 5.9 % 1.5 % 2.1 % 0.5 % 2.5 % 1.6 % - - Accuracy (%) 91.4 % 91.0 % 98.6 % 95.0 % 86.0 % 95.8 % 96.8 87.8 QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.27 28.2 1465 7656 0.392 1.61 - - Precision (%) 5.5 % 4.1 % 1.9 % 1.4 % 2.4 % 4.7 % - - Accuracy (%) 92.7 % 93.9 % 97.7 % 95.7 % 87.4 % 96.4 % - - THCV Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.0143 0.303 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.7 28.1 1488 7371 0.0116 0.224 - - Precision (%) 2.6 % 2.3 % 1.1 % 0.5 % 4.9 % 0.8 % - - Accuracy (%) 86.6 % 93.5 % 99.2 % 92.1 % 81.0 % 88.7 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.3 29.1 1548 7579 0.0117 0.213 - - Precision (%) 4.2 % 1.3 % 1.2 % 1.1 % 5.4 % 1.0 % - - Accuracy (%) 92.9 % 96.8 % 103.2 % 94.7 % 81.9 % 84.5 % - - Batch-3 n 6 6 6 6 6 6 1 1 Av. 9.4 27.7 1523 7339 0.0119 0.211 - - Precision (%) 4.4 % 2.4 % 0.7 % 0.6 % 4.3 % 0.5 % - - Accuracy (%) 94.0 % 92.5 % 101.5 % 91.7 % 83.5 % 83.8 % 99.1 104.1 QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.12 28.3 1520 7430 0.0117 0.216 - - Precision (%) 5.2 % 2.8 % 1.9 % 1.7 % 4.8 % 2.7 % - - Accuracy (%) 91.2 % 94.3 % 101.3 % 92.9 % 82.1 % 85.7 % - - THCVA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.0728 0.446 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.7 27.5 1467 7455 0.0686 0.423 - - Precision (%) 1.2 % 1.5 % 0.6 % 0.7 % 1.6 % 1.0 % - - Accuracy (%) 86.9 % 91.6 % 97.8 % 93.2 % 94.2 % 94.7 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.2 28.9 1521 7569 0.0675 0.405 - - Precision (%) 2.9 % 1.4 % 0.9 % 0.7 % 1.9 % 1.6 % - - Accuracy (%) 91.8 % 96.2 % 101.4 % 94.6 % 92.7 % 90.7 % - - Batch-3 n 6 6 6 6 6 6 1 1 Av. 9.2 27.8 1535 7363 0.0695 0.411 - - Precision (%) 1.9 % 1.1 % 0.6 % 0.6 % 1.7 % 0.7 % - - Accuracy (%) 91.6 % 92.8 % 102.3 % 92.0 % 95.4 % 92.1 % 101.1 102.5 QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.01 28.1 1508 7462 0.0685 0.413 - - Precision (%) 3.3 % 2.5 % 2.1 % 1.3 % 2.0 % 2.2 % - - Accuracy (%) 90.1 % 93.5 % 100.5 % 93.3 % 94.1 % 92.5 % - - CBDV Precision, Accuracy and Recovery QC Sample QC-LLOQ(ng/mL) QC-1 (ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.188 0.0415 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 9.0 28.0 1474 7648 0.175 0.0389 - - Precision (%) 3.0 % 2.6 % 1.5 % 1.7 % 1.9 % 3.6 % - - Accuracy (%) 90.3 % 93.5 % 98.3 % 95.6 % 93.4 % 93.7 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.2 28.8 1517 7732 0.170 0.0372 - - Precision (%) 2.7 % 2.0 % 1.5 % 0.9 % 1.1 % 2.7 % - - Accuracy (%) 92.3 % 95.9 % 101.1 % 96.7 % 90.2 % 89.6 % - - Batch-3 n 6 6 6 6 6 6 1 1 Av. 9.3 27.9 1520 7361 0.169 0.0368 - - Precision (%) 3.9 % 2.4 % 0.6 % 1.4 % 0.9 % 2.1 % - - Accuracy (%) 93.3 % 93.0 % 101.3 % 92.0 % 89.9 % 88.7 % 96.7 98.6 QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.20 28.2 1504 7580 0.171 0.04 - - Precision (%) 3.4 % 2.6 % 1.8 % 2.5 % 2.2 % 3.7 % - - Accuracy (%) 92.0 % 94.1 % 100.2 % 94.8 % 91.2 % 90.7 % - - CBDVA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) Cannabis CRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.719 0.126 (%) (%) Batch-1 n 6 6 6 6 6 6 - - Av. 8.8 27.5 1453 7560 0.714 0.111 - - Precision (%) 2.1 % 1.0 % 1.6 % 1.8 % 1.8 % 2.6 % - - Accuracy (%) 88.1 % 91.5 % 96.9 % 94.5 % 99.2 % 88.3 % - - Batch-2 n 6 6 6 6 6 6 - - Av. 9.1 28.5 1503 7666 0.695 0.108 - - Precision (%) 2.1 % 1.2 % 1.3 % 1.0 % 0.7 % 5.6 % - - Accuracy (%) 90.6 % 94.9 % 100.2 % 95.8 % 96.7 % 86.1 % - - Batch-3 n 6 6 6 6 6 6 1 1 Av. 9.2 28.1 1534 7422 0.711 0.112 - - Precision (%) 2.0 % 1.1 % 1.2 % 1.2 % 2.1 % 0.9 % - - Accuracy (%) 92.3 % 93.5 % 102.3 % 92.8 % 98.9 % 88.6 % 104.2 100.0 QC sample Inter-Batch Stats n 18 18 18 18 18 18 - - Av. 9.03 28.0 1497 7549 0.707 0.110 - - Precision (%) 2.8 % 1.8 % 2.6 % 1.9 % 2.0 % 3.6 % - - Accuracy (%) 90.3 % 93.3 % 99.8 % 94.4 % 98.3 % 87.7 % - - CBL Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) CannabisCRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.0741 - (%) (%) Batch-1 n 6 6 6 6 6 - - - Av. 8.6 27.5 1460 7531 0.0662 - - - Precision (%) 1.3 % 1.4 % 0.7 % 0.7 % 0.7 % - - - Accuracy (%) 86.0 % 91.8 % 97.3 % 94.1 % 89.3 % - - - Batch-2 n 6 6 6 6 6 - - - Av. 8.9 28.9 1515 7648 0.0638 - - - Precision (%) 1.9 % 1.1 % 0.6 % 0.7 % 1.1 % - - - Accuracy (%) 89.0 % 96.3 % 101.0 % 95.6 % 86.1 % - - - Batch-3 n 6 6 6 6 6 - 1 1 Av. 9.0 27.2 1490 7423 0.0637 - - - Precision (%) 1.7 % 1.1 % 0.6 % 0.6 % 0.8 % - - - Accuracy (%) 90.2 % 90.7 % 99.3 % 92.8 % 86.0 % - 96.8 94.7 QC sample Inter-Batch Stats n 18 18 18 18 18 - - - Av. 8.84 27.9 1488 7534 0.0646 - - - Precision (%) 2.6 % 2.9 % 1.6 % 1.4 % 2.0 % - - - Accuracy (%) 88.4 % 92.9 % 99.2 % 94.2 % 87.1 % - - - CBLA Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) CannabisCRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 0.187 - (%) (%) Batch-1 n 6 6 6 6 6 - - - Av. 8.6 27.6 1508 7768 0.205 - - - Precision (%) 2.7 % 2.5 % 3.7 % 3.2 % 1.6 % - - - Accuracy (%) 86.4 % 92.1 % 100.5 % 97.1 % 109.7 % - - - Batch-2 n 6 6 6 6 6 - - - Av. 9.6 29.4 1501 7715 0.193 - - - Precision (%) 2.3 % 1.0 % 1.6 % 0.6 % 1.3 % - - - Accuracy (%) 95.9 % 97.9 % 100.0 % 96.4 % 103.1 % - - - Batch-3 n 6 6 6 6 6 - 1 1 Av. 9.2 27.4 1514 7369 0.197 - - - Precision (%) 3.3 % 2.6 % 2.4 % 1.7 % 1.9 % - - - Accuracy (%) 92.4 % 91.4 % 100.9 % 92.1 % 105.4 % - 101.2 91.3 QC sample Inter-Batch Stats n 18 18 18 18 18 - - - Av. 9.16 28.1 1508 7617 0.198 - - - Precision (%) 5.1 % 3.7 % 2.6 % 3.1 % 3.1 % - - - Accuracy (%) 91.6 % 93.8 % 100.5 % 95.2 % 106.1 % - - - Δ8-THC Precision, Accuracy, and Recovery QC Sample QC-LLOQ(ng/mL) QC-1(ng/mL) QC-2(ng/mL) QC-3(ng/mL) HempCRM(mg/g) CannabisCRM(mg/g) HEMPRRSRecovery CannabisRRSRecovery 10 30 1500 8000 - - (%) (%) Batch-1 n 6 6 6 6 - - - - Av. 8.7 27.9 1467 7500 - - - - Precision (%) 1.5 % 1.5 % 0.8 % 0.6 % - - - - Accuracy (%) 87.5 % 93.0 % 97.8 % 93.8 % - - - - Batch-2 n 6 6 6 6 - - - - Av. 9.2 29.3 1524 7667 - - - - Precision (%) 2.4 % 0.8 % 0.7 % 0.7 % - - - - Accuracy (%) 92.2 % 97.7 % 101.6 % 95.8 % - - - - Batch-3 n 6 6 6 6 - - 1 1 Av. 9.1 27.4 1494 7465 - - - - Precision (%) 2.3 % 0.9 % 0.3 % 0.6 % - - - - Accuracy (%) 91.0 % 91.5 % 99.6 % 93.3 % - - 98.1 95.7 QC sample Inter-Batch Stats n 18 18 18 18 - - - - Av. 9.02 28.2 1495 7544 - - - - Precision (%) 3.0 % 3.1 % 1.7 % 1.3 % - - - - Accuracy (%) 90.2 % 94.1 % 99.7 % 94.3 % - - - - Repeatability and Intermediate (Int) Precision of Cannabinoids in Seven Cannabis Samples ID THC THCA CBD CBDA CBG CBGA CBN CBNA CBC CBCA THCV THCVA CBDV CBDVA CBL CBLA Conc (mg/g) 1 6.26 51.4 4.37 93.2 0.721 3.15 0.123 0.845 0.422 5.25 0.051 0.407 0.020 0.428 <0.002 0.00914 Repeatability (%) 9.2 7.6 8.9 8.8 7.1 9.8 6.5 5.5 3.9 9.8 6.2 7.8 1.8 6.7 N/AP 7.8 Int Precision (%) 7.1 6.1 8.5 5.9 7.1 7.8 5.6 4.3 5.0 6.9 5.3 6.5 6.8 6.5 N/AP 8.0 Conc (mg/g) 2 26.9 26.0 18.1 67.6 0.474 1.80 0.02 0.762 1.46 4.08 0.204 0.210 0.0700 0.282 0.0021 0.0218 Repeatability (%) 3.6 4.6 3.6 4.0 3.5 4.3 5.1 3.6 4.9 4.5 4.9 3.3 6.2 4.1 8.5 10.0 Int Precision (%) 4.4 3.9 4.0 3.7 4.2 4.1 4.2 5.2 5.7 5.9 4.6 3.7 4.9 4.5 10.0 9.3 Conc (mg/g) 3 6.92 124 0.010 0.275 0.726 2.18 0.155 2.36 0.092 0.973 0.034 0.569 <0.002 0.0024 <0.002 <0.002 Repeatability (%) 3.4 4.7 4.4 5.4 4.0 5.3 4.5 4.6 2.0 10.3 3.1 2.6 N/AP 5.4 N/AP N/AP Int Precision (%) 6.1 5.9 8.1 7.6 7.4 8.0 11.0 7.4 8.8 10.7 8.0 6.8 N/AP 11.9 N/AP N/AP Conc (mg/g) 4 5.27 166 0.00736 0.361 1.05 3.83 0.020 0.515 0.159 3.04 0.0133 0.279 <0.002 <0.002 <0.002 <0.002 Repeatability (%) 3.1 2.1 8.8 2.8 1.7 2.2 1.5 2.6 2.9 5.1 12.4 3.8 N/AP N/AP N/AP N/AP Int Precision (%) 8.9 8.1 12.8 6.5 7.2 8.1 7.4 8.7 5.5 7.0 11.0 7.1 N/AP N/AP N/AP N/AP Conc (mg/g) 5 0.917 4.89 9.26 141 0.391 1.29 0.024 0.0643 0.678 6.49 0.0103 0.0576 0.0830 1.38 <0.002 <0.002 Repeatability (%) 6.5 4.0 5.6 6.3 4.7 7.5 1.2 7.0 7.7 7.0 5.8 2.2 1.9 5.9 N/AP N/AP Int Precision (%) 5.2 3.8 5.5 4.4 3.8 5.4 3.6 5.1 5.4 5.5 4.4 2.2 3.6 4.8 N/AP N/AP Conc (mg/g) 6 0.803 5.16 9.31 151 0.636 2.53 0.035 0.113 0.755 7.91 0.00267 0.0157 0.0226 0.362 0.0079 0.0655 Repeatability (%) 2.6 3.2 3.4 1.6 3.6 3.1 3.9 4.5 2.7 5.4 5.6 3.3 5.2 4.4 3.6 3.7 Int Precision (%) 4.6 4.5 5.7 3.8 4.3 4.8 4.2 4.2 4.9 5.2 8.2 8.8 5.6 4.3 3.7 10.8 Conc (mg/g) 7 6.69 13.9 0.00867 0.0462 0.063 0.380 0.129 0.251 0.284 0.551 0.0436 0.104 <0.002 <0.002 <0.002 <0.002 Repeatability (%) 4.8 4.8 6.8 8.1 5.3 4.6 7.6 7.2 3.9 7.8 6.0 6.1 N/AP N/AP N/AP N/AP Int Precision (%) 5.5 4.9 8.7 6.3 4.3 5.4 4.6 6.3 4.4 5.8 4.8 4.7 N/AP N/AP N/AP N/AP ;