Subject: Preparation of standard solution of FECNT



Approved by:____________________________ Initial___________ Date:________

Victor W Pike, Ph.D

Chief, NIMH, PET Radiopharmaceutical Sciences

Batch # PBR-___________ Date_____________

1. Validation of analytical HPLC system ( SOP # QA303; part1 )

|Column: Onyx (monolithic C18; 4.6 mm x 100 mm; Phenomenex; part # CH0 7643) |

|Eluent: Isocratic: 0.01 M ammonium formate in water-acetonitrile (70: 30 v/v) |

|Flow rate: 6 mL/min |

|UV Detector: 220 nm |

HPLC calibration curve:

Y = Mx

where x = peak area via computer integration of UV peak (220 nm) corresponding to PBR28 and Y = (g of PBR28

M = _________ based on calibration curve constructed on ____/____/___

Does injection of 0.300 (g of PBR28 standard on analytical HPLC system give peak area ( 10% of expected peak area based on calibration curve?

Circle one: Yes or No (show calculations below)

Expected peak area = Y/M = 0.300/_____________= _______________

Expected peak area range ( 10% = ___________ –______________

Measured peak area = __________ ; file name: __________________ (attach chromatogram)

2. Validation of Ionization Chamber in Hot-Cell 4

Cs-137 source reference # 970-31-4 204 (Ci on 3/1/2003

Expected radioactivity on date of this test _________ (Ci on _____ (use Excel spreadsheet on bench top HPLC computer)

Acceptable range of radioactivity ____________ –_____________ (use Excel spreadsheet)

Measured radioactivity _______ (Ci on _________ (Remember to push Cs-137 button)

Does measured radioactivity fall within acceptable range (( 5%)?

Circle one: Yes or No

Co-57 source reference #: ___________; ________ mCi on ______/_______/________

Expected radioactivity on date of this test _________ mCi on _____ (use Excel spreadsheet on bench top HPLC computer)

Acceptable range of radioactivity ____________ –_____________ (use Excel spreadsheet)

Measured radioactivity _______ mCi on _________ (Remember to push Co-57 button)

Does measured radioactivity fall within acceptable range (( 5%)?

Circle one: Yes or No

3. Radioconcentration (see SOP # QA301 for sampling for QC)

Withdraw 0.1 ml aliquot from the pyrogen free test tube described in SOP # QA301.

Measure the radioactivity of 0.1 mL aliquot of formulated, sterile-filtered [11C]PBR28 for Injection

_________ mCi at _______

in hot-cell 4 ionization chamber (push C-11 button)

Does measured radioactivity fall within acceptable range of 0.2 to 2.5 mCi?

Circle one: Yes or No

4. Radiochemical Purity, Radiochemical Identity, Specific Radioactivity and Chemical Purity (SOP QA #301)

Inject 0.1 mL aliquot of known radioactivity (see 3) onto HPLC analytical system. Record UV and radioactivity traces. File name: ________________________ (attach chromatogram)

For radiochemical purity criterion, is the radioactivity peak area corresponding to [11C]PBR112 at least 95% of the total radioactivity area in the chromatogram?

Circle one: Yes or No

For radiochemical identity criterion, is the retention time of [11C]PBR28 within ( 0.5 min of that of an injected standard sample of PBR28 (see 1)?

Circle one: Yes or No

tR of standard PBR28 _______ min; tR of [11C]PBR28_______ min

For specific radioactivity test, examine the integrated UV chromatogram and enter the peak area corresponding to carrier PBR28 in the appropriate Excel spreadsheet. Attach the specific radioactivity worksheet to the QC form.

Measured specific radioactivity (end of synthesis): ________ mCi/μmol at ___________

For specific radioactivity criterion, is the specific radioactivity at end of synthesis at least 500 mCi/(mol?

Circle one: Yes or No

Does the integrated UV trace show the area of carrier PBR 28(tR ca. 3.5 min) to be at least 90% of the total UV peak area between 1.5 and 5 min excluding peaks that can be attributed to the formulation vehicle?

Circle one Yes or No

If yes, the 90% chemical purity criterion is met and the maximum allowed volume per injection is determined by the (g/mL of carrier PBR 112. If no, the chemical purity criterion of no more than 1 (g of PBR28 equivalent impurity per administration should be invoked. Using the Excel spreadsheet entitled “PBR28 dose equivalent impurity calculator,” determine the impurity PBR28 dose equivalent/mL. Attach the Excel spreadsheet to the quality control form.

5. pH

Dispense one drop of [11C]PBR 28 for Injection on pH paper (EM Science Catalog # 9578).

Read pH: ________Does measured pH of [11C]PBR 28for Injection fall within the acceptable range of 4.5 to 7.5?

Circle one: Yes or No

6. Appearance Test

Examine the contents of the [11C]PBR28 for Injection dose vial using tongs to hold the dose vial. Is the PET drug product free of particulate matter and is the solution colorless?

Circle one: Yes or No

7. Summary of results of tests that must be completed before release of [11C]PBR 28for Injection

|TEST |Pass or Fail (circle one) |

|Membrane filter Integrity1 |Pass Fail |

|Radioconcentration |Pass Fail |

|Radiochemical purity |Pass Fail |

|Radiochemical identity |Pass Fail |

|Specific radioactivity |Pass Fail |

|Chemical purity |Pass Fail |

|pH |Pass Fail |

|Appearance Test |Pass Fail |

1See production batch record

Time of [11C]PBR28 for Injection product expiration: _______________

This batch passes all specifications of product formulation (print-outs attached):

Chemist __________________________Initials__________________ Date_____________

Batch # PBR-____________ Date_____________

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