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This copy belongs to: Richard Lay, DIO, Division of Food Safety, FDACS 

SOP No. CR CUSTODY 120 Page 1 of 7 

TITLE: Sample/Extract Storage, Holding Times, and Disposal - State and PDP Samples 

Revision: 4 Replaces: 11/30/2006 Effective: 03/06/2009 

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1. Purpose 

To provide standard procedures for the storage, archiving and disposal of state program 

and Pesticide Data Program (PDP) samples and sample extracts. 

2. Scope 

This Standard Operating Procedure (SOP) will be used in the Bureau of Chemical 

Residue Laboratories, Division of Food Safety, Florida Department of Agriculture and 

Consumer Services that are conducting studies for the PDP program. 

3. Outline of Procedures 

6.1 SAFETY PRECAUTIONS 

6.2 Sample Rejection Criteria 

6.3 General 

6.4 Sample Storage Locations 

6.5 Extract Storage Locations 

6.6 Holding Times Prior to Homogenization 

6.7 Holding Times for Unhomogenized Sample Reserves 

6.8 Holding Times for Homogenized Sample Portions 

6.9 Holding Times for Extracts 

6.10 Sample / Extract Disposal 

4. References 

a. USDA SOP, PDP-LABOP-01, Sample Receipt, Storage, Archiving, and Disposal 

b. USDA SOP, PDP-LABOP-03, Sample Preparation for Fresh Fruit and Vegetable, 

Grain, Fish, and Processed Commodities 

c. SOP deviation memo from Diana Haynes to Gail Parker, dated 3/23/04, concerning 1) 

transferring some homogenates to higher temperature freezer (section 6.4.c) and 2) 

releasing blank homogenates to serve as QC matrix (section 6.8.a). 

5. Materials and Apparatus, Media and Reagents, and Associated Documents 

a. Worksheet CR-03025, Initial Sample Log-In 

b. Worksheet CR-03023, Freezer Custody Log 

c. Worksheet CR-03021, Initial Sample Preparation Log 

Bureau of Chemical Residue Laboratories, FL Dept of Agriculture & Cons Services






d. Worksheet CR-04065, Extract Refrigerator Storage Log 

e. Freezer, -40 o C or below 

f. Freezer, -20 o C or below 

g. Refrigerator, not to exceed 4 o C 

h. Cabinet, dry, room temperature, with lock 

6. Specific Procedures 

6.1 SAFETY PRECAUTIONS 

Samples that are shipped with dry ice should be handled using freezer gloves since 

they may be very cold and could cause burns. 

6.2 Sample Rejection Criteria – see CR Custody 110, “Sample Receipt” 

6.3 General 

a. Movement of samples and extracts in/out of storage locations shall be 

documented using appropriate log(s), listed in section 5. 

b. In the Freezer Custody Log (Worksheet CR-03023) each individual freezer 

storage cup, or sample portion, shall have its own log entry. 

c. Samples and extracts shall be stored under lock and key. All freezers, coolers 

and other sample storage areas shall be locked to prevent unauthorized entry. 

d. Some METHOD SOPs may include special storage location, time, and/or 

temperature criteria that are more stringent than listed in this SOP. If so, the 

specific METHOD SOP takes precedence. 

6.4 Sample Storage Locations 

a. Store unhomogenized portions of samples in locations able to maintain status: 

1. Frozen commodities – freezer, -20 o C or below 

2. Fresh, perishable commodities – refrigerator 

3. Packaged, shelf-stable, commodities – cabinet, room temperature 

Note: In certain instances, the locations may differ from those listed in 6.4.a. 

For example, PDP Bananas may be stored at room temperature if they are not 

ripe enough to peel when they are first received. For PDP commodities, consult 

PDP-LABOP-01 and PDP-LABOP-03 for commodity-specific instructions. 







b. Prior to first-time sample extraction, store homogenized portions of samples in 

the -40 o C freezer. 

c. After a sample has been extracted, reserve homogenates may be transferred to a 

higher temperature freezer (e.g.-20 o C) if all the -40 o C freezers are full. 

However, reserve homogenates for violative samples shall remain stored in - 

40 o C freezers. 

6.5 Extract Storage Locations 

Final sample extracts (i.e. extracts ready for instrumental analysis) shall be held in 

refrigerator before and after injection. 

6.6 Holding Times Prior to Homogenization 

Note: Instructions for Initial Sample Preparation of PDP and state regulatory 

samples are in CR METHOD 130 and CR METHOD 131 respectively. 

a. State regulatory samples shall be homogenized on the day of receipt or on the 

next business day. 

b. Fresh PDP commodities may be held up to 72 hours prior to being 

homogenized. 

c. Processed PDP commodities (i.e. canned, frozen) may be homogenized any 

time within the following constraints: 

1. Canned commodities shall be stored unopened until just prior to 

homogenization. Storage may be at room temperature or in a refrigerator, 

but not in a freezer. 

2. Frozen commodities that have not thawed in transit (i.e. still cold to the 

touch) shall be held in the freezer until the sample is homogenized. 

3. Frozen commodities that have thawed in transit (i.e. not cold to the touch) 

shall be refrigerated. If possible, the sample should be homogenized within 

24 hours. However refrigeration of the thawed commodity for a period not 

to exceed 72 hours is acceptable. 

d. Non-routine, Consumer Complaint, and special project samples shall be held 

similarly to PDP samples above unless alternate instructions are provided in 







writing. 

6.7 Holding Times for Unhomogenized Sample Reserves 

a. Non-violative whole commodity reserves (state samples) shall be held in the 

cooler at least 10 working days past the sample extraction date, or until 

CRLIMS QA signoff (if that occurs in less than 10 days). 

Note: PDP samples are homogenized in their entirety, so there are no retained 

unhomogenized portions in the cooler. 

EXCEPTION: State watermelon samples – unhomogenized portions may be 

discarded immediately (especially when many samples are collected during 

watermelon surveys). Due to their size it is difficult to store them in a manner 

that prevents cross contamination of the interior flesh. 

b. Violative whole commodity reserves (state samples) shall be held in the cooler 

at least 10 working days past the sample extraction date, but shall NOT be 

discarded without consultation with the TPM or Bureau Chief. 

Note: PDP samples are homogenized in their entirety, so there are no retained 

unhomogenized portions in the cooler. 

c. Non-routine, Consumer Complaint, and special project whole commodity 

reserves shall be held in the cooler at least 10 working days past the sample 

extraction date, but shall NOT be discarded without consultation with the TPM 

or Bureau Chief. 

6.8 Holding Times for Homogenized Sample Portions 

a. Non-violative freezer homogenates shall be held in the freezer until written 

release following CRLIMS QA signoff. EXCEPTION – Homogenates of an 

analyzed sample may be used as QC matrix blanks prior to written release 

provided that sample contains no reportable analytes and the instrument section 

analysts verify the sample is suitable for use as a matrix blank. The freezer log 

shall reflect the homogenate was used for matrix. 

b. Violative freezer homogenates shall be held in the -40 o C freezer for a minimum 

period of 6 months past the date of CRLIMS QA signoff. The Bureau Chief or 

designee may specify (in writing) an alternate retention date. 

c. Non-routine, Consumer Complaint, and special project freezer homogenates 







shall be held in the -40 o C freezer for a minimum period of 6 months past the 

date of CRLIMS QA signoff. The Bureau Chief or designee may specify (in 

writing) an alternate retention date. 

6.9 Holding Times for Extracts 

a. The instrument sections shall retain sample extracts until after QA CRLIMS QA 

signoff. Extracts may be held longer for special purposes (e.g. special studies, 

UAR libraries, etc). 

b. Any instrument injections made from sample extracts more than 2 weeks old 

shall NOT be used for quantitative purposes without TPM approval. 

Consideration for approval may include, but is not limited to, storage stability 

information. Recalculations of spikes and process controls may help establish 

storage stability. 

6.10 Sample / Extract Disposal 

a. Disposal of samples and extracts shall be documented using appropriate log(s), 

listed in section 5. 

b. The Sample Custodian is responsible for disposal of whole commodity and 

homogenized portions. 

c. The Sample Custodian is responsible for saving and maintaining a supply of 

released blank homogenates to be used as future QC matrix. 

d. Discard whole and homogenized sample portions into plastic bag in trash can. 

e. The instrument section supervisors are responsible for disposal of extracts 

retained by an instrument section. 

f. Discard final and intermediate sample extracts into the appropriate hazardous 

waste stream. Instrument sections deliver extracts contained in reusable 

glassware to Sample Prep section for disposal and glassware cleaning, and 

discard extracts contained in disposable glassware directly into the appropriate 

hazardous waste stream. 







___________________________________________ 

Reviewed By: Gail Parker 

Quality Manager 

Date:_________________ 

Bureau of Chemical Residue Laboratories 

3125 Conner Blvd., Tallahassee, FL 32399-1650 

850-488-9670 

___________________________________________ 

Approved By: JoMarie Cook 

Chief 

Date:________________ 

Bureau of Chemical Residue Laboratories 

3125 Conner Blvd., Tallahassee, FL 32399-1650 

850-488-9670 







REVISION HISTORY: 

Rev Date Description Author(s) 

0 04/02/04 Replaces retired CR Custody 20. Incorporates all holding 

times previously described in retired CR Method 30 and 

retired CR Method 31. 

1 02/18/05 Deleted text “or until at least six weeks after extraction” 

from the first sentence of Section 6.9.a. Extracts must now 

be held until after QA review. This change is in response 

to Corrective Action 2005-03. 

J Gramling 

G Parker 

G Parker 

2 11/28/05 Added requirement for reprepping spikes to section 6.9.c. G Parker 

3 11/30/06 Changed the word ‘form’ to ‘worksheet’ throughout 

document. Added PDP-LABOP-03 to Section 4. Added 

worksheet CR-03024 to Section 5. Added Antibiotic log to 

Section 6.3.b. Added 6.3.d (pertaining to more stringent 

requirements in certain Method SOPs). Added note to 

Section 6.4.a. Added note to Section 6.9.c. Updated 

signature page. 

G Parker 

4 03/06/09 Worksheet CR-03024, Antibiotic Custody, Freezer and 

Cooler log, was removed from the associated documents. 

Updated USDA SOP title. Updated terminology: i.e. 

“CRLIMS QA signoff” instead of “QA Review.” Updated 

approval authority in section 6.9.b and c. Updated position 

titles and other terminology throughout. Deleted obsolete 

instructions pertaining to intermediate extracts. 

Incorporated SOP deviations (multiple) for the retention of 

unhomogenized state watermelon samples. 

J Gramling 

G Parker

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