Document OzLg0dzbqRQn4jQrn3y8Yvzpw
JUN 1 * fiSt
To : J. Edward Fattlar From: Lance A. Mayer
ResljksDAP Extractions
cc:
Keith L. Gardner Bob K. Hinderer
Bernie C. Knoble Bud Pazur
Ashok Shah D'Lane L. wisner Roman W. Wypart File
June lo, isi
summaryr Higher than normal conversion Geon 3400 was used to make a "Mystique" bottle compound with 25 parts of Geon 3400. The bottles were extracted with both 8% ethanol in water and 50% ethanol in water. No residual DAP was found in the extract. The test had a detection limit of 50 parts per billion (ppb).
Discussion; In order to get FDA approvability for the "Mysitic" resins, the resin was modified to obtain a lower residual diallyl phthalate (DAP) level. The modification involved running the reaction to a 15 psi pressure drop rather than the usual 3 psi pressure drop. This was expected to increase the conversion approximately 5%. In the one polymerization made under these conditions, the extra 12 psi pressure drop took one hour to obtain.
A sample of the slurry was obtained and dried in the dryer at the Technical Center. The resin was then compounded by Roman Wypart into the 87536 formulation using 25 parts of Geon 3400 rather than the conventional 20 parts used in the current "Mystique" compound. Earl Price then blowmolded the 12 ounce bottles from this compound to be used in the extraction study.
Brenda Bennett then extracted the bottles using 8% ethanol and 50% ethanol to simulate contact with aqueous foods and alcoholic foods following the protocol in "Guidelines for Migration Studies for FDA Acceptance of Indirect Food Additives" by Wellman C. Bachtel, January 29, 1990. These extractions extended over the course of 10 days. For the first two hours the bottles were stored in a convection oven at 150F. For the rest of the time the temperature was maintained at 120*F. Samples were removed from the three bottles at 2, 8, 24, 48, 96 and 240 hours.
A modification of Dave Ernes's procedure was initially used. This new procedure involved the evaporation of the water and ethanol, re-dissolution in acetonitrile and then analysis via high pressure liquid chromatography. This produced acceptable results in the validation study of the 50% ethanol/water (see Table 1). However, it was discerned that in the samples that were allowed to evaporate overnight (namely the 8% ethanol), an appreciable amount of the DAP also evaporated. This was despite its very low vapor pressure of
22470001
)
BFG21007
about 0.001 mm Hg at ambient temperature. water at 70F is 18.8 mm Hg).
(The vapor pressure of
A procedure was then developed that permitted the analysis of 'the extract directly. (This approach had been abandoned earlier because of the interference of the methanol that was in the ethanol.) This gave acceptable results in the validation, (see Tables 2 and 3).
Experimenta1: Calibration standards were prepared by dilution of DAP into both 8% and 50% ethanol solutions. Standard curves were prepared based on peak height (see Figures 1 and 2) Peak height correlated better than area due to baseline determination.
Prior to injection, the extracts were filtered through a 0.45 m Gelman filter. The following chromatographic conditions were used:
Column: Mobile phase: Flow rate: Injection Vol: Detection:
Varian Reverse Phase C18,
45/55 acetonitrile/water 1.8 ml/min 20fil
UV at 220 nm.
MCH-NCAP-5/x
Figure 3 is the chromatogram of a direct injection of 50% ethanol. Figure 4 shows the chromatogram of a direct injection of the 240 hour extraction sample of a bottle (no peak attributed to the DAP). Figures 5, 6 and 7 show the validation chromatograms where the 240 hour extract sample was spike with 50, 100 and 150 ppb of DAP to determine the recovery percentage. The peak attributed to the DAP had a retention time of '6.3 minutes. Figures 8 through 12 show similar chromatograms for the 8% ethanol.
Conclusions:. Geon 3400 should be FDA approvable where the contents are 0 to 50% ethanol in water or for contact with fatty foods.
since the amount 6t time required for the extra 12 psi pressure drop was inordinately long (an extra hour of polymerization time), the polymerization should be repeated. If it remains this long, the initiator system should be reviewed as well as the possibility of repeating the extraction on normal Geon 3400.
Acknowledgments: I am indebted to: Brenda Bennet for her expeditiously getting this testing done; Daren Whetstone for arranging the polymerization and obtaining the resin; Roman Wypart and Earl Price for making the compound and bottles; and
22470002
BFG2I008
}
Table 1 Percent Recovered from 50% Ethanol/Water Extract
Evaporation Technique
ppb
Results
Average
150 100
50
82.3 98.8 103
84.8 79.9 65.3
84.8 89.4 65.3
84.0 89.4 77.9
Table 2 Percent Recovered from 50% Ethanol/Hater Extract
Direct Analysis Technique
ppb
Results
Average
150 100
50
99.4 74.4 74.0
94.4 104.3
74.0
99.4 104.3
59.1
97.7 94.3 69.0
Table 3 Percent Recovered from 8% Ethanol/Water Extract
Direct Analysis Technique
ppb
Results
Average
150 100
50
84.9 73.8 84.0
90.0 86.4 98.8
100.1 79.0 83.9
91.7 79.7 88.9
) BFG21009
Peak Height
Ftgur* 1
DAP CALIBRATION in 8% EtOH
DAP (ppb)
| Ftflur2 ]
DAP CALIBRATION
> BFG21010
Peak Height
\n W L V Z Z
0 FIGURE 3
CHANNEL A
INJECT 06/94/91 09:43:50 STORED TO BIN * 88
J
FIGURE 4
CHA1MEL A
S7>c?c cK.
S'-3 ja.t/o Aa'> +
INJECT 06/94/91 13:99:99 STORED TO BIN 199
BFG21011
DAP EXTR 8 SOX VWfet-P
FILE 9.
METHOD 0.
06/94/9199:43:59
RUN 87
INDEX 26
PEAKI
HTX
RT PK HT BC
1
9.792
0.67
571 02
.2
(.42
0.81
(924 92
9
1 .595
|
1995 92
4
0.192
1.87
1B9 92
5
0.133
1.49
96 92
6
9.126
1.41
91 93
7
9.985
3.14
61 91
9
99.991
4.29 64999 99
9
6.79
5.24
4999 95
10
0.921
7.31
IS 92
11
9.942
9.99
39 93
12
9.913
9.69
9 91
TOTAL
199.
72997
CH "A* PS* 1. BIN 89
WARN INC - HEHORY AT 1. K - UNPROTECTED CWMATOCRMS HILL BE REPLACE
smaLVZZ
DATA SAVED TO BIN 199
DAP EXT8 0 SOX VALIDATION
96/94/91 13:99:99
FILE 8.
METHOD 9.
RUN 99
INDEX 38
PEAKI
HTX
RT PK HT BC
1
1.46
0.63
1013 02
2
1.592
9.91
1043 02
9
1.419
1.
984 02
4
0.246
1.37
171 92
5
0.25
1.52
173 02
6
9.127
1.62
09 93
7
9.923
2.6
16 02
9
0.921
2.79
15 93
9
944
3.54
28 01
10
99.167
4.26 61988 08
11
5.799
5.22
3963 05
12
9.036
0.02
25 01
TOTAL
199.
69497
CH *A* PS- I . BIN 1B0
HARMING - MEMORY AT 0.X- UNPROTECTED CHROMATOCRAHS HILL BE REPLACED
HARMINC " ntdUHY Al O. K - UfU'KUILUtU OWUNAIUUKAnS HILL BE REPLACED
jtflit. J Sl,y *- - - ''* ***'''
FIGURE S
CHANNEL A
*3 S-Ofr*
INJECT 06/04/91 15:03:24 STORED TO BIN S 103
^cuuso-*r/>i, ~>*p
CHANNEL A
INJECT 06/34/91 16:22:41 STORED TO BIN t IOS
DATA SAVED TO BIN I 103
DAP EXT* SOX VALIDATION
06/04/91 15:03:24
FILE 3.
METHOD 0.
RUN 102
INOEX
PEAKS
HTX
RT PK HT BC
1
1.34
9.66
096 02
2
1.503
0.0
1005 02
3
I .460
0.99
901 02
4
0.14
1.26
93 02
5
0.263
1.35
176 02
6
0.179
1.47
120 02
7
0.104
1.61
69 08
0
0.104
2.00
69 02
9
0.076
2.57
51 02
10
0.092
3.49
61 03
II
09.665
4.21
59960 08
12
4.937
5.17
3301 OS
IS
0.046
6.27
81 01
14
0.032
7.63
22 02
15
0.052
0.08
as oa
TOTAL
100.
6637.1
Ctt> *A* PS- 1 .
9000LVZZ
DATA SAVED TO BIN t 105
DAP EXTR 50% VALIDATION
06/04/91 16:22:41
FILE 8.
WTHOD 0.
RUN 104
INDEX 43
PEAKS
HTX
RT PK HT BC
1
0.106
0.12
77 01
2
0.473
0.38
347 01
8
2.697
0.66
1976 02
4
2.523
0.8
1040 02
5
2.264
0.99
1659 02
6
0.630
1.36
584 02
7
0.404
1.40
355 02
0
0.106
2.11
77 03
9
0.04
2.62
29 02
10
0.0S8
2.78
48 02
11
0.076
8.56
96 03
12
05.672
4.28 62763 08
18
4.696
5.23
8440 05 , , , ,
14
0.00
6.32
59 g|tt* /6 /-It {S'-
15
0.087
8.1
27 01
TOTAL
100.
73259
CH= "A* PS- 1.
UABNINC NEHORV AT 2. K UNPROTECTED CHROMATOGRAMS HILL BE REPLACED
BFG21012
CHANNEL ft
'pt/. ,.< c * f vi^u4--c *td/V>/. ZW/''
INJECT 06/05/71 11:I<:3$ STORES TO BIN 3 111
3^--*--
.37 1.40
OAP EXTR * 502 WftUPftTJON
06/05/71 If. 21:35
FILE 3.
KETWOO B.
RUN 110
1NOEX 47
PEAK*
t
Z 3
4
5 6 7 0 P 10
11 12 13
14
15 16
total
HU
B.I63 334 3 .JP5
3.132 2.660
0.521
0.46 0.037
002
0.B3I 0.P0 0.033 5.575 3.466 0.126 0.041
t00
RT PK MT BC
0.36
0.40 0.67
0.0 0.P7 1.37
1.40
2.05
2.74 3.03 3.16
3.59 4.32 5.1?
6.44
0.01
107 02
217 03 2157 02
2051 02 1747 2 341 02 801 2
24 03 13 02
20 02
64 02 21 02 56024 00
2267 05 ,
a 0i *:
27 01
65460
* *ft* pSM } . BIN 11)
/oooUKZ
extr e so* validation
FILE 0.
METHOD 0.
PEAK*
I
Z 3 4 5 6 7
a
9
10
11 12 13
total
KTX
0.575 1.682 M.371 0.637
1.172
0.192 0.271 0.154 71.713 0.747 0.067 0.077 0.067
100.
l
0.IZ 0.38 0.64 0.77 1.37 1.65 3.17 3.73 4.32 5.28 5.70 7.42 0.14
06/05/71 12:14:*j
**** "Z
INDEX SI
PX HT Sc
24 03 34 02 17 02 8783 08 117 05
01
10 02 0 03
12525
WARNING -
INK LOU -
CH= 'ft* ps_ ,
BIN Kg
l0 lZ O d g
tS-v
CHANNEL A
riUUAG. 7
AVoiOO*
W* A?A
INJECT 06/05/91 M: 17:51 STORED TO BIN t 122
FIGURE 10
DATA SAVED TO BIN B 122
DAP EXTR 0 50X VALIDATION
06/05/91 14:17:51
FILE 8.
METHOD 9.
RUN 121
INDEX 60
PEAK!
HTX
RT PK HT 8C
1
29.174
0.67
3957 82
2
P.27P
9.P8
1259 82
3
2.292
1.53
299 83
4
0.246
2.74
33 82
S
8.216
3.09
29 82
6
8.265
4.01
36 82
7
58.544
4.20
7941 83
8
8.074
6.92
10 01
TOTAL
180.
13565
PS 1 . BIN 122
WARNING - MEMORY AT 9. K - UNPROTECTED CHROMATOGRAMS WILL BE REPLACED INK LOU - CHANCE PRINT CARTRIDGE AND PRESS CCTlt-SHIFT-Cl
8VWM/HZ
DATA SAVED TO BIN t 9
DAP EXTR 82 VALIDATION
FILE 6
.METHOD 0
06/11/Pl 11:16:33
RIM 136
INDEX 75
PEAKS
HTX
RT PK HT BC
1
0.697
0.39
77 02
.2
1 .537
0.46
171 83
8
17.654
0.66
1960 82
4
18.663
0.98
2872 09
5
0.576
8.14
64 05
6
59.293
4.25
6583 01
7
0.724
6.3
80 02 v
8
0.231
7.1
26 02
9
0.261
7.79
29 02
10
0.267
8.62
30 02
11
0.096
9.5
11 03
TOTAL
100.
11102
CH= 'A' PS- 1 . BIN 9
, ,. ,v
-
WARNINC - MEMORY AT 0. K - UNPROTECTED CHROMATOGRAMS HILL BE REPLACED INK LOU - CHANCE PRINT CARTRIDGE AND PRESS CCTRL-SHIFT-C3
BFG21014
FIGURE 11
74*C" /(-O/pb
CHANNEL A
INJECT 06/85/91 16:17:28 STORED TO BIN S 128
J
ROURE 12
CHANNEL A
~ ^41 s^rrl`
INJECT 06/85/91 15:18:00 STORED TO BIN a 125
BFG21015
DATA SAWED TO BIN a 128
Tit
DAP EXTR 9J*Z VALIDATION
86/85/91 16:17:28
FILE 8.
METHOD 0.
RUN 127
INDEX 66
PEAKa
HTX
RT PK NT BC
1 2 3 4 5 6 7 8 9 18 11
TOTAL
8.529 8.959 19 .697 6.559 1 .175 8.685 8.225 69.625 8.117 8.362 8.866
fOO.
0.39
8.48 6.66 8.98 1 .37
1.51 2.82 4.32 5.26 6.42 7.79
72 82 131 82 2683 82 893 82 168 82
93 83 31 82 9483 83 16 01 49 8I<
9 81
13620
/
CH* *A* PS 1 . BIN 128
/- -
WARNING - MEMORY AT 2.X- UNPROTECTED CHROMATOGRAMS HILL BE REPLACED INK LOH - CHANCE PRINT CARTRIDGE AND PRESS CCTRL-SHIFT-CJ
60003
DATA SAVED TO BIN 8 125
fv7
DAP EXTR MX VALIDATION
86/05/91 15:16:00
FILE 8. PEAK!
METHOD 8.
HTX
RT
RUN 124
INDEX 63
PK HT BC
1
8.592
0.12
67 81
2
1.219
0.37
137 82
3
17.664
8.64
1989 82
4
6.725
8.96
757 08
5
0.178
1.51
28 85
6
0.124
3.86
14 82
7
72.995
4.29
8221 03
8
8.302
6 .38
34 81
V'
9
0.124
8.56
14 82
18
8.877
9.2
9 03
TOTAL
180.
11262
CH= *A* PS= 1. BIN 125
'' j, , ->
WARNING - MEMORY AT 1. K - UNPROTECTED CHROMATOGRAMS WILL BE REPLACED INK LOU - CHANCE PSIHT CARTRIDGE AND PRESS CCTRL-SHIFT-C3
BFGoodrich
The BFGoodrich Company
3925 Embassy Parkway Akron, Ohio 44333-1799
FAX:
216-374-2333 216-374-2238
216-374-3338 216-374-3456
1st Floor 2nd Poor
3rd Floor Legal
DATE:
June 4, 1991
TO: Chuck Purks ALTC
V'
~aJi
PHONE: Fax: 933-1678
NUMBER OF PAGES:
1 (INCLUDING COVER PAGE)
COMMENTS: RE: GEON 86155 TRANS 0025
Please check the following:
1) I cannot confirm that Synpron 221 is FDA acceptable I cannot find trisnonylphenyl phosphite in any of the sections quoted: 181.29,181.27,178.2010. The supplier should be asked under what section(s) would Synpron 221, and not the individual components, be cleared. Also, under what section Is TNPP cleared?
2) The supplier for POS7 does not list 181.27, a Prior Sanction for EPLSO. Does this product meet ZICFR specs: iodine number maximum 6; oxlrane oxygen, minimum 6 percent? WU they certify that It meets 21CFR 181.27?
T O O U V rc
FROM:
Bob Hinderer__________ BFGoodrich - Corporate
PHONE: 374-4534
*/l JJP
BFG21016
