File TUSS.BK

Directory of image this file is from
This file as a plain text file








                                 .SP

                       .CE          DEPARTMENT


    .CE        PHENYLPROPANOLAMINE HYDROCHLORIDE    18.75 MG/5 ML
    .CE        CHLORPHENIRAMINE MALEATE               2.0  MG/ 5ML




                                 .SP2

         
                 IS  DETERMINED  BY  COLORIMETRIC   REACTION   WITH
         TETRAHYDRODIMETHOXYFURANE
                 AND  P-DIMETHYLAMINOBENZALHYDE  USINGA  "TECHNICON
         AUTOANALYSER". THE
                 CHLORPHENIRAMINE    MALEATE(SK&F    1223I)     AND
         CARAMIPHEN ETHANEDISULFONATE
                 (TORYN-SK&F   769J)   ARE   DETERMINED  ON  A  GAS
         CHROMATOGRAPH USING
                 A 6'  3% OV17 COLUMN.

         
                 AN AUTOMATED ANALYTICAL SYSTEM CONSISTING  OF  THE
         FOLLOWING
                 

         
                 FLASK,DISSOLVE   COMPOUND   IN   ABOUT  75  ML  OF
         DEIONIZED WATER AND DILUTE
                 TO VOLUME WITH THE SAME


                 FLASKS. DILUTE TO VOLUME WITH WATER.
                 2.4 SAMPLE PREPARATION
                 PIPET 2.0 ML OF SAMPLE INTO A  100  ML  VOLUMETRIC
         FLASK, ADD ABOUT 75 ML OF DEIONIZED
                 MIX AND DILUTE TO VOLUME WITH THE SAME SOLVENT.
                 NEAR ZERO ABSORBANCE HAS BEEN ESTABLISHED.
                 TRANSFER   THE  THREE  WORKING  STANDARDS  TO  THE
         SAMPLING TRAY OF THE SAMPLER
                 EQUIPPED WITH NOMINAL 8.5 ML SAMPLING CUPS. IN THE
         SAME MANNER
                 , TRANSFER THE SAMPLE  PREPARATION  TO  THE  TRAY.
         PROGRAM
                 THE SAMPLER AT A RATE OF 20/HR  WITH A 20-1/2 CAM,
                 AND  IN  SUCH  A  FASHION  THAT  THE STANDARDS ARE
         REDETERMINED AT THE
                 END OF THE RUN.
         
                 SUBTRACT VALUE OF THE STEADY STATE BASELINE(A ).









                                                                   2






                 AVERAGE THE FACTORS OBTAINED (F    ).  THE  FACTOR
         AT EACH POINT
                 SHOULD NOT VARY FROM THE AVERAGE BY MORE THAN  +/-
         5%.

         
                 OF THE STEADY STATE BASELINE (A  ).


                 





                 .        2.63 CLAIM  18.75 MG SK&F 11A / 5 ML

                         3.0   DETERMINATION OF SK&F 1223I AND SK&F
                 769J
                         3.1  REAGENTS
                              SKELLYSOLVE F (SKELLY PETROLEUM CO.)
                              PHENIRAMINE  MALEATE   (SK&F   1224I)
                 INTERNAR STANDARD.
                              USE  A  CONCENTRATION OF ABOUT 5 MG /
                 ML
                              1 N  SODIUM HYDROXIDE
                         3.2  STANDARD PREPARATION
                              ACCURATELY WEIGH ABOUT 200 MG OF SK&F
                 769J AND 40 MG
                              OF  SK&F  1223I   INTO   A   100   ML
                 VOLUMETRIC FLASK, DISSOLVE
                               IN   AND   DILUTE   TO  VOLUME  WITH
                 DEIONIZED WATER. PIPET 4.0
                              ML OF THIS  SOLUTION  INTO  AN  8  ML
                 SCREWCAP VIAL,PIPET
                              IN   SUCCESSIVELY   1.0   ML  OF  THE
                 INTERNAL STANDARD AND
                              2.0 ML OF THE  SKELLSOLVE  F.  ADD  2
                 DROPS OF THE SODIUM
                              HYDROXIDE  SOLUTION,CAP  TIGHTLY  AND
                 AGITATE WITH A
                              VORTEX  MIXER  FOR  ABOUT  1  MINUTE.
                 ALLOW THE PHASES
                              TO SE

                              

                         3.3   SAMPLE PREPARATION
                                SUBSTITUTE  4.0  ML  OF  SAMPLE  IN
                 PLACE OF THE









                                                                   3


                                 STANDARD SOLUTION  AND PROCEED  AS
                 DIRECTED ABOVE
                                 IN 3.2.
                         3.4   CHROMATOGRAPHY

                                  INSTRUMENT    PERKIN  ELMER MODEL
                 881
                                  COLUMN       6 FT GLASS(1/8 IN.)-
                 3% OV17
                                                ON    GASCHROM    Q
                 100/120 MESH
                                  COLUMN TEMPERATURE    190 C
                                  FLOW  RATE  40 ML/MIN
                                  INJECTION VOLUME   2 MICROLITERS
                                  CHART SPEED  4 MIN / INCH
                                  ATTENUATION 100X
                                  INTEGRATOR  IF AVAILABLE
                               INJECT    2   MICROLITERS   OF   THE
                 SKELLYSOLVE PHASEINTO
                               THE   CHROMATOGRAPH.    START    THE
                 INTEGRATOR AFTER
                               THE  SOLVENT  HAS ELUTED AND THE PEN
                 HAS RETURNED
                               ALMOST TO BASELINE.

                         3.5   CALCULATIONS
                               IF  USING  PEAK  HEIGHTS,   DRAW   A
                 BASELINE TANGENT TO
                               THE  BEGINNING  AND END OF EACH PEAK
                 AND MEASURE ITS
                               HEIGHT ABOVE THIS BASELINE. IF USING
                 AN INTEGRATOR
                               USE THE AREA PRINTED  OUT  FOR  EACH
                 PEAK.

                               CALCULATE  RESPONSE FACTORS FROM THE
                 STANDARD SAMPLE
                               DATA.


                                 P  /P     X  C    = F


                                 P  /     X  C    =   F

                               WHERE:  P    = AREA OR  PEAK  HEIGHT
                 OF INTERNAL STANDARD
                                       P     =  AREA OR PEAK HEUGHT
                 OF SK&F 769J
                                       P    = AREA OR  PEAK  HEIGHT
                 OF SK&F 1223I
                                       C    = CONCENTRATION OF SK&F
                 769J
                                       C    = CONCENTRATION OF SK&F









                                                                   4


                 1223I
                                       F     =  RESPONSE  FACTOR OF
                 SK&F 769J
                                       F    =  RESPONCE  FACTOR  OF
                 SK&F 1223I


                              FOR   EACH   SAMPLE   CALCULATE   THE
                 CONCENTRATION OF EACH
                              COMPONENT AS FOLLOWS:


                                 F  X  P   /    X 5  =     MG  SK&F
                 769J/5 ML

                                 F   X  P   /P   X 5  =     MG SK&F
                 1223I/ 5 ML


                              WHERE:  P    = AREA OR PEAK HEIGHT OF
                 SK&F 769J
                                      P    = AREA OR PEAK HEIGHT OF
                 SK&F 1223I

                         3.6 METHOD VALIDATION

                         3.61  TORYN   EDISYLATE(SK&F   769J)   AND
                 CHLORPHENIRAMINE
                              MALEATE(SK&F 1223I).
                              USING  A PLACEBO SYRUP AND A STANDARD
                 SOLUTION OF THE
                              ACTIVE   INGREDIENTS   5    REPLICATE
                 DETERMINATIONS
                              WERE MADE.
                              RESULTS:

                                  SK&F 769J            SK&F 1223I
                                  2.069 MG/ML           0.432 MG/ML
                                  2.007                 0.431
                                  2.088                 0.411
                                  2.026                 0.414
                                  2.035                 0.428

                         THEORY   2.020                 0.410
                         AVERAGE  2.045                 0.423
                         S.D. +/- 0.033                 0.009
                         REL SD ;/- 1.6%                 2.1%
                         RECOVERY 101.1%                101.2%

                         3.62   PHENYLPROPANOLAMINE   HYDROCHLORIDE
                 (SK&F 11A)
                              NO RECOVERY  DATA  WAS  OBTAINED  FOR
                 THIS PARTICULAR
                              FORMULATION BUT SIMILIAR PREPARATIONS









                                                                   5


                 IN THE TUSS-
                              ORNADE   REFORMULATION  PROGRAM  GAVE
                 100.9% RECOVERY
                              WITH  A  STANDARD  DEVIATION  OF  ;/-
                 1.1%.
                                    



Feel free to contact me, David Gesswein djg@pdp8online.com with any questions, comments on the web site, or if you have related equipment, documentation, software etc. you are willing to part with.  I am interested in anything PDP-8 related, computers, peripherals used with them, DEC or third party, or documentation. 

PDP-8 Home Page   PDP-8 Site Map   PDP-8 Site Search