Quality Control Samples

 

DEPARTMENT OF HEALTH

RULE NO.:RULE TITLE:

64ER20-10Quality Control Samples

SPECIFIC REASONS FOR FINDING AN IMMEDIATE DANGER TO THE PUBLIC HEALTH, SAFETY OR WELFARE: Pursuant to Chapter 2019-116, § 41, at 31, Laws of Florida, the Department is not required to make findings of an immediate danger to the public, health, safety, or welfare.

REASON FOR CONCLUDING THAT THE PROCEDURE IS FAIR UNDER THE CIRCUMSTANCES: The Department of Health is directed by Chapter 2019-116, § 41, at 31, Laws of Florida, to adopt emergency rules to implement section 381.988, Florida Statutes.

SUMMARY: Emergency rule 64ER20-10 addresses the use of quality control samples by CMTLs.

THE PERSON TO BE CONTACTED REGARDING THE EMERGENCY RULE IS: Courtney Coppola at [e-mail].

 

THE FULL TEXT OF THE EMERGENCY RULE IS:

 

64ER20-10 Quality Control Samples

(1) CMTLs must use Quality Control samples in each analysis, where applicable. Quality Control samples must be analyzed in the same manner as Testing Samples for validation purposes. The following Quality Control samples must be in each analysis for Mycotoxins, Residual Solvents, Heavy Metals, Agricultural Agents, and Cannabinoid Profile:

(a) CMTLs must prepare at least one Method Blank sample per Laboratory Batch. All Method Blank samples must be prepared and analyzed in the same manner as Testing Samples. Method Blanks that contain Target Analytes above the Limit of Detection must be reanalyzed. If upon reanalysis the Method Blank is again above the Limit of Detection the CMTL must determine and correct the source of the contamination, repeat the preparation of the Laboratory Batch, and reanalyze the Testing Samples. If Method Blank results continue to read above the Limit of Detection, the CMTL must discontinue conducting the analysis until such time it is able to test at or below the Limit of Detection.

(b) CMTLs must prepare and analyze Laboratory Fortified Blanks for each Laboratory Batch. The percent of recovery for any Target Analyte within each Laboratory Fortified Blank, calculated as the quantitative sample result ÷ expected result × 100, must be recorded. The CMTL must determine acceptable ranges of recovery in Laboratory Fortified Blanks which must be approved within the scope of the CMTL’s ISO 17025 accreditation. If the concentration of Spike Solution is lower than the expected concentration in a submitted sample, spiking post dilution is permitted.

(c) CMTLs must prepare and analyze Matrix Spike Samples for each Laboratory Batch. The percent of recovery for any Target Analyte within each Matrix Spike Sample, calculated as the quantitative sample result ÷ expected result × 100, must be recorded. The CMTL must determine acceptable ranges of recovery in Matrix Spike Samples which must be approved within the scope of the CMTL’s ISO 17025 accreditation. If the concentration of Spike Solution is lower than the expected concentration in a submitted sample, spiking post dilution is permitted.

(d) CMTLs must run duplicate Laboratory Fortified Blanks and Matrix Spike Samples and must calculate their Relative Percent Differences (RPD). RPD is calculated as (quantitative sample result A – quantitative sample result B) ÷ ((quantitative sample result A + quantitative sample result B) ÷ 2) × 100. The RPD between duplicates must be as follows;

1. Mycotoxins: 20% or less;

2. Residual Solvents: 30% or less;

3. Heavy Metals: 20% or less;

4. Agricultural Agents: 20% or less; and

5. Cannabinoids: 15% or less.

(e) CMTLs shall run an Initial Calibration Verification (ICV) after the Calibration Curve, and Continuing Calibration Verification (CCV) after the ICV, and once every 12 hours, or at a minimum, every 10 samples, thereafter in the analysis run. The CMTL shall calculate the RPD between the ICV and the corresponding Calibration Curve level, and the CCV and the corresponding Calibration Curve level. The RPD between the Calibration Curve level and corresponding CCV or ICV must be no more that 20%.

1. If the CCV results exceeds more than 20% above the corresponding Calibration Curve level concentration, any Target Analyte result below the LOQ may be reported. Otherwise the samples affected by the failed CCV shall be reanalyzed after a new Calibration Curve has been established and accepted.

2. If the CCV result exceeds more than 20% below the corresponding Calibration Curve level concentration, any Target Analyte result above the Acceptable Limits may be reported. Otherwise the samples affected by the failed CCV shall be reanalyzed.

(f) Methods containing multiple Target Analytes may have a representative number of Target Analytes chosen for the required Spike Solution.

1. For Analytical Methods that include one (1) to five (5) Target Analytes, the Spike Solution must contain all Target Analytes

2. For Analytical Methods that include five (5) to 20 Target Analytes, the Spike Solution must contain 50% of the Analytical Method Target Analytes, with a minimum of five (5) Target Analytes.

3. For Analytical Methods that include more than 20 Target Analytes, the Spike Solution must contain a minimum of 16 Target Analytes.

4. The CMTL must ensure all Target Analytes are included in the Spike Solution at least once in a two-year period.

(g) Methods containing multiple Target Analytes may have the following number of Target Analytes in a Quality Control sample fall outside the accepted range to a maximum of 30%:

1. Analytical Methods containing fewer than 11 Target Analytes are allowed no measurements outside the accepted range.

2. Analytical Methods containing 11 to 30 Target Analytes are permitted one (1) Quality Control sample outside the accepted range.

3. Analytical Methods containing 31 to 50 Target Analytes are permitted two (2) Quality Control samples outside the accepted range.

4. Analytical Methods containing 51 to 70 Target Analytes are permitted three (3) Quality Control samples outside the accepted range.

5. Analytical Methods containing 71 or more Target Analytes are permitted four (4) Quality Control samples outside the accepted range.

(h) An analysis will be deemed satisfactory when all Quality Control sample measurements meet the accepted criteria. If any Quality Control sample measurements fall outside the accepted criteria, the Laboratory Batch must be reanalyzed. If after reanalysis the same Quality Control sample falls outside the accepted criteria, the CMTL must repeat the preparation of the Analytical Batch and reanalyze as a new Laboratory Batch. If the Quality Control sample continues to fall outside the accepted criteria, the CMTL must discontinue conducting the analysis until the CMTL is able to correct the cause of the unsatisfactory Quality Control sample measurement.

(i) CMTLs must generate Quality Control sample reports that contain the date of the analysis, the parameters of the analysis, the Matrix or Matrixes used, the Target Analytes tested for, the instrument of analysis, and measurements.

(j) If the number of Analytical Samples in an Analytical Batch for Mycotoxins, Residual Solvents, Heavy Metals, Agricultural Agents, or Cannabinoid Profile is greater than 20, the Analytical Batch must be split between multiple Laboratory Batches such that the Quality Control samples in each Laboratory Batch correspond to a maximum of 20 Analytical Samples.

(2) For Microbiological Testing by quantitative polymerase chain reaction (qPCR), the Laboratory Batch must include one positive Quality Control sample able to detect 1 CFU per gram, one negative Quality Control sample, and one replicate Analytical Sample per Analytical Batch. Microbes with an Acceptable Limit less than 1 CFU per gram must undergo a 24-hour enrichment before testing.

Rulemaking Authority 381.988(3), 381.988(9), FS. Law Implemented 381.988 FS. History–New.

 

THIS RULE TAKES EFFECT UPON BEING FILED WITH THE DEPARTMENT OF STATE UNLESS A LATER TIME AND DATE IS SPECIFIED IN THE RULE.

EFFECTIVE DATE: January 22, 2020