ML20069M231

Forwards Repts Entitled, Investigation Rept on Blind Performance Test Samples, Addressing Three False Negative Blind Tests Recently Experienced

ML20069M231
Person / Time
Site:	Seabrook
Issue date:	06/16/1994
From:	Feigenbaum T NORTH ATLANTIC ENERGY SERVICE CORP. (NAESCO)
To:	NRC OFFICE OF INFORMATION RESOURCES MANAGEMENT (IRM)
References
NYN-94066, NUDOCS 9406210250
Download: ML20069M231 (7)

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Nortli North Atlantic Energy Service Corporation g.O. no,300 o

~ Atlantic se b" " m o3874 (603) 474-9521, Fax (603) 474-2987 The Northeast Utilities Systern Ted C. Feigenbaum NYN. 94066 Senior Vice President &

Chief Nuclear Officer June 16,1994 United States Nuclear Regulatory Commission Washington, DC 20558 Attention: Document Control Desk

Reference:

Facility Operating License No. NPF-86, Docket No. 50-443

Subject:

False Negative Blind Tests

Dear Mr. Bush:

l l North Atlantic Energy Service Corporation (North Atlantic) has enclosed two reports entitled I

" investigation Report on Blind Performance Test Samples." The enclosed reports, prepared by Duo Research, Inc., address three false negative blind tests which were recently experienced. These tests do not constitute unsatisfactory performance on the part of SmithKline Beecham Clinical Laboratories under the IlllS guidelines according to Dr. Robert E. Willette of Duo Research, Inc.

It is our understanding that you wish to be infonned of all false negative tests, regardless of whether or not they constitute unsatisfactory performance.

If you have any questions, or wish any additional information, please feel free to contact Mr.  ;

Bruce Seymour, Security Manag;r at 603-474-9521, extension 4015.

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Very truly yours, l # f "

Ted C. Feigenbaum TCF:ALIlact Enclosures l

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, United States Nuclear Regulatory Commission June 16,1994 Attention: Document Control Desk Page two ec: Mr. Thomas T. Martin Regional Administrator United States Nuclear Regulatory Commission Region 1 475 Allendale Road King of Prussia, PA 19406 Mr. Albert W. De Agazio, Sr. Project Manager Project Directorate I-4 Division of Reactor Projects U.S. Nuclear Regulatory Commission Washington, DC 20555 Mr. Antone C. Cerne NRC Senior Resident Inspector l P.O. Box 1149 Seabrook, Nil 03874 j Mr. Loren L. Bush l Safeguards Branch l USNRC Washington, DC 20555 l

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' North Atlantic June 16,1994 1

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ENCLOSURE TO NYN-9-1066

INVESTIGATION REPORT on Blind Performance Test Samples Objective:

The licensee shall investigate any unsatisfactory performance testing result.

A record shall be made of the investigative findings and the corrective action taken by the labcratory. The licensee shall send the document to the NRC as a report of the unsatisfactory performance testing incident within 30 days. l

References:

1. 10 cra 26 Appendix A, subpart 2.8(e)(4)

2. TR 53, 11970 (1988), subparts 3.19(b)(2) & (5)

Observation:

A blind quality control sample containing a combination of morphine, morphine- '

3-glucuronide, cedeine and 6-acetylaorphine was reported negative by the SmithKline Beecham Clinical Labcratorium = Norriwtown. An unannouncwd Iml>olua tory site visit was conducted by Dr. Robert E. Willette on May 25, 1994.

Findincta s The sample was prepared for submission to the laboratory by the Seabrook site on Harch 23, 1994. llt was roccived by tho laboratory on March 24, 1994, and subjected to the initial immunoassay test on March 25th. The sample gave a positive response in the Emit opiate assay, with a value that use 1.585 timen the cutoff calibrator (300 ng/mL cf morphine) value. The sample was then submitted to the GC/MS confirmatien assay on March 26th. The sample was ana-lyzed for codeine and morphine, obtaining concentrations of 129 and 293 ng/mL, respectively. Although there was a problem noted with one or more control samples by the analyst, the final reviewer determined that this did not con-stitute sufficient cause to repeat the analysis. Since the morphine result was below the cutoff of 300 ng/mL, the sample was reported as negative.

An identica1' sample was submitted by the Seabrook site, which was received by the laboratory on May 13th, and another identical sample was also received on May lith by the laboratory, which was submitted by a different client under DOT testing rules. Both samples gave similar screening values, 1.505 and 1.549, respectively. The May lith por sample gave analytical results of 101 ng/mL of codeine and 240 ng/mL cf morphine, and was reported as negative. The May 13th sample submitted by sembrock pzoducwd results of 109 and 331 ng/mL, respectively. As this result was above the cutoff, it was reported as a positive for morphine.

The average reference values obtained on thio comple wore 112 nghnL for codeine, $22 ng/d for total morphine (119 free morphine plus ca. 500 as the glucuronide), and 61 ng/mL of 6-acetylmerphina.

These results are in contrast to a similar sample (from a previous lot) that was analyzed by the laboratory en February 5, 1994, in which the GC/M5 results were 109 ng/mL of codeine and 615 ng/mL of morphine. Average reference values for this sample were 109 ng/mL of codeine and 597 ng/mL total morphine.

Duo Research Inc.

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Nonh Atlantic Energy Service Corp. page 2 Findings (continuedi The significant drop in total merphine from the earlier sample, together with l thu variable results cbtained with the three latter samples, suggests incom- l plete hydrolysis and recovery of morphine from it natural glucurenide conju- '

gate. However, the laboratory includww high and low control samples that centain a 50:50 mixture of free and conjugated morphine to monitor the hydrol- ,

ycio etep. In ecch of the GC/HC runs reviewed, the recovery of total morphine I from these control samples was within the expected limits. This does not I cernplately rule out the possibility of incomplete hydrolycio of the cample l reported as negative, but the icw recovery of morphine in three identical l samples tested on thr** neparate occasions suggests possible other variables. '

Recommendation l

Although this is an isolated false negative report for morphine, it should be investigated further as two subsequent samples also were found to have quanti-tative results significantly below the average reference value.

Because these samples screened positive and were submitted to confirmation, the laboratory has retained then in frozen storage, which is standard practice fer the laboratory. Therefore, it is recommended that the laboratory reana-lyze the March 25th and May 13th sanples and submit an appropriate aliquot to an outside reference laboratory fer independent analysis. It is suggested that the aliquets be sent to BlSohly Laboratories, Inc., an EH3-certified laboratory that served as one of the reference laboratories for this particular sample lot.

The two samples are identified by the SFCL accession numbers 829182A and 979555A, rc=cived by the laboratory on 3/24/94 and 5/12/94, respectively.

Prepared for North Atlantic Energy Service Corporation by: MFM/CLfk Dates f/ f*/ 27 /19 4 J '

Duo Research Inc.

Duo Research Inc.

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J INVESTIGATION REPORT on Blind Performance Test Samples Objective The licensee shall investigate any unsatisfactory perfomance testing result.

A record shall be made of the investigative findings and the corrective action taken by the laboratory. The licensee shall send the document to the NRC as a report of the unsatisf actory perfomance testing incident within 30 days.

References:

1. 10 CrR 26 Appendix A, Subpart 2.8(e)(4)

2. FR 53, 1197o ( U68), Subparts 3.19(b)(2) E (5)  ;

1 Observations I Two blind quality control samples containing a combination of Tac-9-carboxylic acid (reference value 27 ng/mL) and another cannabinoid, in sufficient concen-tration to produce a positive screening result, were reported negative by thw SmithKline Beecham Clinical Laberatories - Norristown. An unannounced labora-tory site vinit was conducted by Dr. Robert 3. Willette on May 25, 1904.

Findingst l

l These two samples, which are designed to challenge the laboratory near the confimation cutoff of 15 nghrt, were submitted by the Seabrook. site and received by the laboratory en April 29 and May 13, 1994. Both produced poni tive initial test results, giving values in the Emit cannabinoid assay that were 1.163 and 1.176 times the 100 ng/mL cutoff calibrator, respectively, and 3.519 and 3.180 times the 50 ng/mL cutoff calibrator, respectively. Both were submitted to GC/M5 analysis. Although both samples gave quantitative values that were close to the reference value, the analyses were repeated with diluted aliquots because an interfering peak was observed in one of the ion scans, causing it to fail the ion ratio qualifying criteria. similar results were obtained in the repeat analyses, so both samples were reported as negative, which is in accordance with certitication requirements. j It is noted that the cannabinoic confimation procedure utilised by the labor-  !

atory is a standard procedure used in all BBCL certified laboratories. This  ;

investigator has observed similar results with retwwtv conductwd in anothwr SBCL facility, that is, interference in the 488 ion. Ms. Susan Mills, the laboratory responsible person, indicated that the laboratory had minaed a cannabinoid in the most recent National laboratory Certification Program (the kas-oponoored program) maintenance PT curvey. It appcare that the accay procedure does not provide either sufficient " clean up" during the liquid-liquid extraction stop or separation during the chromatography.

. In also noted that a nearly identical suple containing the combination described above has been submitted to the laboratory on several occasions during 1993 and has never been reported as negative. In fact, the samples from the earlier lot had a slightly lower concentration of THC-9-carboxylic acid (reference average 22 ng/mL). Also, the laboratory has correctly identi-fled samples centaining the TEC metabolite at concentrations just above the 100 ng/mL cutoff level.

Duo Recearch Inc.

North Mantic Energy Service Corp. Page 2 Findin09 (continuedit It should also be noted that identical samples as discussed above have been reported correctly by several other laboratories to which they have been uulmaitted as blind oc samples.

It appears t. hat, there may havw been some change in the assay procedure that dess not provide sufficient elimination of interferences at concentrations below 30 ng/mL.

Rocommendations These two results, in and of themoolvoo, do not constituto unoatisfacto n experience under the prevailing regulations. However, the conse:utive misses on these blind QC samples, together with reported miss(es) on NI.cP PT surveys, support the observation that the current confirmation assay may require modi- l fication. It is recccmended that the laboratory be requested to ra-evaluate I its assay procedure for possible changes to improve it perfomance at lower l ccncentrations of the TEC metabolite. Also, the laboratory should be request-ed to provide information about the NLCP maintenance PT survey results mentioned above.

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Prepared fort North Atlantic Energy Service Corporation by: N, /b Dates M f/ N 2 7, /T i V _

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Duo Research Inc.

Duo Research Inc.

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