1. (1) Calibration Standards must be prepared by diluting Certified Reference Materials to produce working standards to be used in the Calibration of instruments, the quantitation of Analytical Samples, and for use in Laboratory Fortified Blanks and Matrix Spike Samples. CMTLs must prepare Calibrations for Agricultural Agents and Mycotoxins in a Matrix that matches the Analytical Batch being tested. Certified Reference Materials must be:

   1. (a) Obtained from an independent body that holds ISO/IEC 17034:2017 accreditation; or
   2. (b) Created by the CMTL, if the CMTL holds ISO/IEC 17034:2017 accreditation; and
   3. (c) Within the manufacturer’s or CMTL-determined expiration date.
2. (2) The LOD must be calculated for Mycotoxins, Heavy Metals, Residual Solvents, Agricultural Agents, and Cannabinoid Profile. In the determination of the LOD, the CMTL must follow the U.S. Environmental Protection Agency, “Definition and Procedure for the Determination of the Method Detection Limit,” Revision 2, December 2016, which is incorporated by reference herein and available at HYPERLINK "https://flrules.org/Gateway/reference.asp?No=Ref-19584"https://flrules.org/Gateway/reference.asp?No=Ref-19584. The LOD for chemical methods must be 1/5 of the Acceptable Limit or less with an instrument signal to noise ratio of 3:1 or greater for each Target Analyte, including all isomers and compounds thereof, as calculated in the Analytical Sample after correction for all Dilution Factors and sample weights or volumes.
3. (3) The LOQ must be calculated for Mycotoxins, Heavy Metals, Residual Solvents, Agricultural Agents, and Cannabinoid Profile. The LOQ for chemical methods must be no lower than the lowest Calibration Standard, and a maximum of ½ of the Target Analyte’s Acceptable Limit as calculated in the Analytical Sample after correction for all Dilution Factors and sample weights or volumes. The LOQ must have a Signal-to-noise Ratio of 10:1 or greater.
4. (4) For Heavy Metals analysis, the instrument detection limit must be measured as the concentration equivalent to the Target Analyte signal which is equal to three (3) times the standard deviation of a series of 10 replicate measurements of the calibration blank signal at the selected analytical mass(es). The instrument detection limit cannot be greater than the LOD. The instrument detection limit samples must be prepared and run in three (3) separate batches over three (3) separate days.

5. (5) The Calibration Curve must:

   1. (a) Use the concentration and percentage for each analyte and isomer identified in the Certificate of Analysis from the ISO/IEC 17034:2017 accredited Certified Reference Material provider to calculate the concentration of all standard curve points.
   2. (b) Consist of a minimum of five (5) consecutive points with a known concentration above zero if utilizing a linear correlation with no non-consecutive points added;
   3. (c) Consist of a minimum of six (6) consecutive points with a known concentration above zero if utilizing a non-linear correlation with no non-consecutive points added;
   4. (d) Consist of a minimum of six (6) consecutive points with known concentrations above zero and utilize a quadratic correlation for Cannabinoid analysis;
   5. (e) Have a response and be integrated in accordance with Rule 64-4.312, F.A.C.; and

   6. (f) Have a correlation of determination (r2) using all standard curve points equal or greater to 0.99.

      1. A CMTL may only use non-linear correlations if linear correlations do not meet the 0.99 r2 requirement.

      2. A CMTL may only use weighted correlations if non-weighted correlations do not meet the 0.99 r2 requirement.

   7. (g) Use calibration table values corresponding with on-instrument concentrations excluding calculations and Dilution Factors;
   8. (h) Have an in-Matrix concentration spanning from, at a minimum, the LOQ to the inhalation limit, no more than three (3) times the inhalation Acceptable Limit for each individual Target Analyte, and, with the exception of Residual Solvents, have a maximum Dilution Factor of 20 for non-inhalation Target Analytes;
   9. (i) Use the same instrument method for all Injections of Calibration Standards, Quality Control Samples, and Analytical Samples;
   10. (j) Have all Calibration Standards be from the same run sequence;
   11. (k) Not have multiple calibration points at the same concentration averaged to create one calibration point at that concentration;
   12. (l) Not be used for samples which were injected before the Calibration Standards used in the Calibration Curve were injected; and
   13. (m) Be the most recently established Calibration Curve used for sample analysis. Quality Control Samples and Analytical Samples may not be analyzed with a previous Calibration Curve once a new Calibration Curve has been established.
6. (6) The highest level on the Calibration Curve shall be the highest reportable value. Any subsequent results greater than the highest level on the Calibration Curve must be diluted and reanalyzed or reported as greater than the highest level on the Calibration Curve.
7. (7) A Calibration Curve is deemed established when the regression is analyzed and compared to the requirements set forth in this rule.

Rulemaking Authority Art. X, § 29, Fla. Const., 381.988(3), 381.988(9) FS. Law Implemented Art. X, § 29, Fla. Const., 381.988 FS. History–New 5-28-26.