headspace grade solvents for trace analysis of organic volatile … · 2020. 9. 21. · –...
TRANSCRIPT
Subhra Bhattacharya, Eric Oliver and Stephen C. Roemer Thermo Fisher Scientific – Fisher Chemical, One Reagent Lane, Fair Lawn, NJ
Headspace Grade Solvents for Trace Analysis of Organic Volatile Chemicals
Material and MethodsAbstract
Headspace GC analysis is a common practice in the pharmaceutical industry to detect residual solvents. Per United States Pharmacopoeia (USP), residual solvents in pharmaceuticals are defined as organic volatile chemicals that are used or produced in the manufacturing of drug substances or excipients. Since residual solvents are difficult to remove completely from drug products, the amount of residual solvent should be evaluated by headspace GC analysis. Based on their toxicity effects, residual solvents are classified as Class 1 (most toxic), Class 2 and Class 3. In headspace GC analysis, the pharmaceutical compound of interest is often dissolved in a high boiling solvent to isolate trace amounts of volatile components. Although water is the most common solvent for this purpose, other solvents can be used when solubility of the pharmaceutical compound is an issue.
We have evaluated five different solvents for headspace analysis. The solvents are water, dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMAC) and 1-methyl-2-pyrrolidone (NMP). The purpose of our study is to qualify these high purity solvents for residual solvent analysis in pharmaceuticals. Four different pain medications were purchased from Walgreens and residual solvent analysis performed using DMSO and water. Our results showed that all five headspace solvents are free of trace level impurities and qualified to detect volatile organic components at trace level from pharmaceutical compounds.
• Solvents: All GC headspace grade solvents were from Thermo Fisher Scientific – Fisher Chemical,Fair Lawn, NJ
GC Headspace
Reagent Fisher Chemical
Grade Pack Size PackagingFisher Scientific
Cat. No
Water GC Headspace 1L amber glass W10-1
DMSO, Dimethyl Sulfoxide GC Headspace 1L amber glass D139-1
DMF, Dimethyl Formamide GC Headspace 1L amber glass D133-1
DMAC, Dimethyl Acetamide GC Headspace 1L amber glass D160-1
NMP, N-methyl Pyrrolidone GC Headspace 1L amber glass N140-1
For more information about these products please visit www.fisherchemical.com
• Standards: Class 1 (catalog # PHR1063) and Class IIA (catalog # PHR1064) residual solvent standard mixfrom Sigma-Aldrich, St. Louis, MO
• Samples: pain medication from Walgreens
1. Ibuprofen
2. Acetaminophen
3. Aleve
4. Aspirin
• Sample preparation:
1. Ten tablets were dissolved in 10 mL of water and the mix centrifuged. Supernatant (2 mL) wastransferred to a 20 mL headspace GC (HSGC) vial.
2. Ten tablets were dissolved in a mixture of water and DMSO (50:50). The mixture was centrifuged and thesupernatant transferred to a 20 mL HSGC vial.
Headspace GC-FID run conditions
• Instrument: Thermo Scientific Trace GC Ultra equipped with headspace RSH auto sampler
– Column: ZB-624, 30 m x 0.25 mm x 1.4 micron
– Detector: flame ionization detector (FID)
– Detector temperature: 250º C
– Injector temperature: 200º C
– Syringe volume: 2.5 mL
– Injection volume: 1.0 mL
– Split ratio: 20
– Agitator temperature: 90º C
– Incubation time: 5 min
– Hydrogen: 35, Air: 350, Nitrogen: 40
– Oven temperature:
Initial 40º C & hold 5 min
Ramp 10º C per min
Final 240º C & hold 10 min
2 3
For a limited time: Buy1 Case, Get 1 Case on GC HeadSpace sovlents! Please visit: www.fishersci.com/solventsale to redeem today!
Results and DiscussionResults and Discussion
• Headspace GC-FID run of Class 1 and Class IIA residual standards (without any dilution) in DMSO isshown in Fig. 1. All five peaks of the Class 1 residual solvent mixture were detected using the method; the14 peaks from the Class IIA residual solvent mixture were also detected in the same method. The residualsolvent peaks are eluted before the DMSO peak (at 10.27 minutes).
• Fig. 2 shows an overlay of the expanded chromatograms of DMSO solvent with Class 1 residual solventstandard mix, namely 1 – 5 ppm concentration, 100 – 500 ppm concentration, and the Class IIA standardmix at 100 – 1600 ppm concentration. This data clearly shows that there are no trace amounts ofextraneous peaks present in the HSGC solvent.
• Class IIA residual solvent standard mix was diluted further, and the final concentration of components werewithin the 1 – 16 ppm range. A comparison of this lower concentration standard mix relative to the DMSOblank shows a clean solvent baseline without interference from extraneous peaks (Fig. 3).
• Figs. 4 – 7 show the blank HSGC-FID run of each solvent and the Class 1 and Class IIA standards in thesame solvent. No extraneous peaks were observed in any of the solvents.
• An HSGC-FID analysis of all four pain medications is provided in Fig. 8. Some common peaks wereobserved in all samples; only in the Aleve solution a peak at 8.40 minutes was found different than theother samples.
• Fig. 9 provides the HSGC-MS spectra of the 8.40 min peak from Aleve sample (run in a different columnusing a different method).
• An HSGC-FID analysis of a toluene standard at 1 ppm concentration showed the same retention as theunknown peak in Aleve samples. Moreover, GC-MS spectra of the unknown peak and toluene standard areidentical, which confirms the presence of toluene in the Aleve material. However, the amount of toluene inAleve is less than 1 ppb, which is much lower than the recommended level of USP (Fig. 10).
Figure 1. Class 1 and Class 2 Solvent Standards by GC-FID Headspace
Class 1 solvents mix Full scalefigure 1RT: 0.00 - 25.02
0 2 4 6 8 10 12 14 16 18 20 22 24Time (min)
0
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Cou
nts
2.38
6.17
5.63
6.26
10.27
7.412.511.56 9.370.14 5.062.93 16.0715.52 16.71 17.677.57 18.8014.37 20.50 21.09 22.2010.74 23.5012.20
8.2710.01
1.55
5.65
10.279.68
7.125.323.25
9.504.842.81
7.4124.7323.9122.6221.4419.3918.5917.3616.5515.6714.346.18 13.5410.732.400.99 9.154.72
NL:4.28E5Channel 2 Analog 2 Class-I_residual-solvent-standard-01
NL:1.61E5Channel 2 Analog 2 class-iia_residual-solvent-standard-01
RT: 0.04 - 10.99
1 2 3 4 5 6 7 8 9 10Time (min)
020000400006000080000
100000120000140000160000
050000
100000150000200000250000300000350000400000
Cou
nts
2.38
6.17
5.63
6.26
10.275.86 7.412.51 10.361.56 9.371.280.14 5.062.930.45 4.852.02 3.28 3.83 4.03 6.976.39 7.57 8.03 8.41 8.75 9.57
8.27 10.01
1.555.65
10.279.689.587.125.323.259.504.842.81 7.416.182.400.99 8.371.72 9.157.746.400.17 4.723.34 4.33
NL:4.28E5Channel 2 Analog 2 Class-I_residual-solvent-standard-01
NL:1.61E5Channel 2 Analog 2 class-iia_residual-solvent-standard-01
Class 2 solvents mix
Expanded 1-1 1-2
1-4
1-3
1-5
2-1
2-2 2-3
2-4 2-5
2-6
2-7
2-8 2-9 2-11
2-10
2-12
2-14
2-13
1-1 – 1,1-Dichloroethene1-2 – 1,1,1,-Trichloroethane1-3 – Carbon tetrachloride1-4 – Benzene1-5 – 1,2-Dichloroethane
2-1 – Methanol2-2 – Acetonitrile2-3 – Methylene chloride2-4 – Trans-1,2-Dichloroethene2-5 – Cis-1,2-dichloroethane2-6 – Tetrahydrofuran2-7 – Cyclohexane2-8 – Methylcyclohexane2-9 – 1,4-Dioxane2-10 – Toluene2-11 – Chlorobenzene2-12 – Ethylbenzene2-13 – m-Xylene, p-xylene2-14 – o-Xylene
Figure 2. DMSO Neat, Class 1 and Class IIA Standard MixRT: 0.05 - 11.10
1 2 3 4 5 6 7 8 9 10 11
Time (min)
0
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Cou
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4000
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10.31
0.98 10.580.14 9.47 10.179.271.19 2.20 8.877.651.74 8.457.422.49 3.03 6.863.44 3.67 4.61 6.394.14 5.01 5.23 6.12
10.319.321.00 6.13 8.442.38 5.581.58 9.508.22 8.897.306.966.735.290.16 4.854.483.863.443.141.94
2.40 6.175.63
9.356.265.86 10.490.99 9.51 9.957.442.52 9.220.16 8.918.307.716.514.531.28 7.002.17 3.04 4.951.73 3.49 4.30 5.47
9.679.58
3.25
5.34 9.504.832.95
10.369.362.82 7.410.990.14 9.121.73 7.506.20 6.823.83 4.38 4.94
NL:4.39E4Channel 2 Analog 2 DMSO_headspace_100to1
NL:1.89E5Channel 2 Analog 2 class-i_1-5ppm_hsfid_20to1_in_dmso
NL:4.86E4Channel 2 Analog 2 class-i~100-500ppm_83to1split_in_dmso
NL:4.64E4Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_dmso
DMSO blank
Class 1 standard (1 – 5ppm in DMSO)
Class 1 standard (100 – 500 ppm in DMSO)
Class IIA standard (100 – 1600 ppm in DMSO)
Figure 3. DMSO and Class IIA Standard Mix at Lower Concentration
Class IIA standard mix (1 – 16 ppm)in DMSO
BlankDMSO
4 5
Results and DiscussionResults and Discussion
Figure 4. DMAC Neat, Class 1 and Class IIA Standard Mix Figure 5. DMF Neat, Class 1 and Class IIA Standard Mix
RT: 0.01 - 9.57
1 2 3 4 5 6 7 8 9Time (min)
05000
1000015000
20000250003000035000
40000
05000
1000015000200002500030000350004000045000
Cou
nts
0
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15000
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25000
30000
35000
40000
0.970.15 0.69 1.48 1.72 2.612.02 2.77 3.20 3.47 3.80 4.28 8.887.69 8.554.56 8.037.104.78 6.865.31 5.53 6.456.00
2.40 6.185.64 6.270.990.37 9.197.44 8.918.572.521.28 8.277.867.151.89 4.203.29 3.85 5.264.49 4.91
7.12
8.261.553.25 5.334.832.952.82 7.420.99 8.987.49 8.350.16 1.25 6.541.70 6.795.872.05 3.42 4.293.760.53
NL:2.93E5Channel 2 Analog 2 N,N-DMF_headspace_100to1
NL:3.32E5Channel 2 Analog 2 class-i~100-500ppm_83to1split_in_nn-dmf
NL:3.03E5Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_nn-dmf
Expanded
DMF blank
Class 1 standard
Class 1 standard
Class IIA standard
Class IIA standard
DMF blank
RT: 0.00 - 11.28
0 1 2 3 4 5 6 7 8 9 10 11
Time (min)
4500
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6500
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9000
0.970.17 10.539.580.48 1.10 9.351.96 10.048.608.367.732.49 7.522.72 7.146.723.16 3.90 6.335.874.21 4.48 5.59
2.40
6.18
5.64
6.27
5.860.99 10.630.15 10.007.452.52 9.598.877.77 8.280.41 1.69 6.57 6.793.692.04 3.35 4.724.13 5.45
5.33
9.679.58
4.83
2.94
9.50
2.827.42
9.380.98 10.609.250.15 1.72 8.142.34 6.460.83 3.32 6.676.193.95 4.47
NL:2.46E5
Channel 2 Analog 2 DMA_headspace_100to1
NL:2.60E5
Channel 2 Analog 2 Class-I~100-500ppm_83to1Split_in_DMA
NL:2.23E5
Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_dma
DMAC blank
Class 1
Class IIA
6 7
Results and DiscussionResults and Discussion
Figure 6. Water Neat, Class 1 and Class IIA Standard Mix
RT: 0.00 - 25.02
0 2 4 6 8 10 12 14 16 18 20 22 24Time (min)
6000
8000
10000
12000
14000
5500
6000
6500
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7500
8000
Cou
nts
6500
7000
7500
8000
8500
21.66 22.34 24.1420.4119.8819.2018.1216.5915.7515.28
14.9914.80
14.6014.39
14.0613.80
13.3412.8510.73
0.99 10.541.02 9.747.03 8.202.33 3.35 4.73 6.706.27
6.17
2.40
5.64
9.3625.0123.2921.5420.5519.5718.5618.0616.0415.6514.5213.5310.400.99 12.397.442.52 9.281.28 5.034.14
10.008.26
1.56
5.333.25 9.504.83 5.652.95
7.122.82 24.6123.6722.8021.6019.8219.2418.1717.1016.057.42 10.29 15.0214.3113.230.99 9.341.75 7.013.35
NL:8.73E3Channel 2 Analog 2 headspace_water_v-2
NL:8.47E3Channel 2 Analog 2 class-i~100-500ppm_83to1split_in_water
NL:1.56E4Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_water
RT: 0.06 - 10.50
1 2 3 4 5 6 7 8 9 10Time (min)
6000
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6500
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8000C
ount
s
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6080
6100
6120
6140
6160
6180
62000.99
0.140.31
0.4210.34
1.02 10.189.741.29 9.287.031.57 8.708.208.142.33 6.93 7.832.39 3.15 3.35 3.67 4.733.98 4.79 6.705.21 6.266.24
6.276.17
2.40
5.64
9.36
5.86 10.400.99 9.527.442.52 9.280.16 7.62 8.968.011.28 6.543.010.70 5.03 6.801.52 2.34 4.143.37 4.593.7210.008.26
1.56
5.333.25 9.504.83 5.652.95
7.122.82 7.42 10.290.990.16 9.431.75 8.777.951.270.49 2.51 7.013.35 3.89 6.614.27 5.905.24
NL:6.20E3Channel 2 Analog 2 headspace_water_v-2
NL:8.47E3
Channel 2 Analog 2 class-i~100-500ppm_83to1split_in_water
NL:1.56E4Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_water
Class 1 standard
Class IIA standard
Water blank
Expanded from 1-10 minutes
Figure 7. NMP Neat, Class 1 and Class IIA Standard Mix
Class 1 standard
Class IIA standard
NMP blank
Expanded
RT: 0.00 - 13.76
0 1 2 3 4 5 6 7 8 9 10 11 12 13Time (min)
0
10000
20000
30000
40000
50000
0
10000
20000
30000
40000
50000
Cou
nts
0
10000
20000
30000
40000
50000
12.11
13.7012.200.97 10.37 12.000.16 11.129.524.363.923.58 8.241.21 7.95 8.642.54 6.874.692.14 6.525.62
12.15
2.40 10.296.175.63 6.27 12.25 13.670.99 10.53 11.9410.017.442.520.13 9.058.731.61 8.204.774.413.21
12.15
5.65
7.12
8.261.55 10.0010.283.25 9.675.33 9.574.832.95 7.41 10.36 13.5312.240.99 11.7911.231.720.14 8.996.28 8.156.613.32 4.73
NL:5.68E4Channel 2 Analog 2 N-MP_headspace_100to1
NL:5.33E4Channel 2 Analog 2 class-i~100-500ppm_83to1split_in_n-mp
NL:5.45E4Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_n-mp
Time (min)
RT: 0.08 - 13.69
1 2 3 4 5 6 7 8 9 10 11 12 13
5200
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5800
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Cou
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5400
5600
5800
6000
6200
6400
6600
13.5612.200.97 10.37 12.0011.580.16 9.524.363.923.58 8.241.21 9.297.952.54 6.874.692.14 6.525.62
6.27
12.25 13.670.99 10.53 11.9410.017.442.52 9.950.13 9.058.731.61 7.13 8.202.832.26 4.774.41 5.033.98
2.82
7.41
13.5312.249.42 10.490.99 11.799.231.720.14 7.506.28 6.612.53 3.32 4.733.92
NL:5.68E4Channel 2 Analog 2 N-MP_headspace_100to1
NL:5.33E4Channel 2 Analog 2 class-i~100-500ppm_83to1split_in_n-mp
NL:5.45E4Channel 2 Analog 2 class-iia_100-1600ppm_83to1split_in_n-mp
Figure 8. Headspace Analysis of Pain Medications by GC-FID (Expanded)RT: 0.08 - 10.96
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5Time (min)
6000
6500
7000
7500
8000
8500
9000
9500
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5800
5900
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6700
6800
Co
un
ts
5600
5700
5800
5900
6000
6100
6200
6300
6400
6500
6600
670010.68
3.043.45 10.298.501.44 9.13 10.099.718.568.468.187.685.35 7.377.136.766.476.145.403.551.76 5.184.764.501.78 4.292.06 2.620.20 1.360.930.80
10.682.04
3.04
10.54
3.441.771.44 10.2910.098.19 9.569.198.707.667.496.806.475.363.572.89 5.92 7.094.020.84 2.22 5.034.17 4.770.35 1.11
10.46
2.04
10.68
3.041.77 3.441.45 8.19 10.299.123.54 7.955.36 8.56 9.967.20 9.667.576.775.99 6.512.942.26 5.844.27 5.200.26 4.541.290.880.63
NL:6.73E3Channel 2 Analog 2 81315_water_acetaminophen_1
NL:6.85E3Channel 2 Analog 2 81415_dmso_acetaminofen_filtered_1
NL:1.09E4Channel 2Analog 281415_dmso_acetaminophen_nf2
RT:0.00 - 10.39
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0Time (min)
58006000
6200640066006800700072007400
760078008000820084008600
570058005900600061006200630064006500660067006800690070007100
Cou
nts
8.40
3.03
3.441.44 10.211.772.04 5.330.16 3.55 4.20 4.52 5.432.662.47 5.010.710.51 5.75 9.871.02 9.136.11 7.056.33 6.84 9.757.49 8.31 8.937.76
2.04
8.40
3.041.771.44 3.430.120.35 0.91 2.271.33 2.65 3.54 8.184.423.88 4.98 5.324.59 5.675.92 10.296.116.436.677.007.277.517.74 9.12 10.208.49 9.58
NL:7.15E3Channel 2 Analog 2 81315_water_aleve_1
NL:8.65E3Channel 2 Analog 2 81415_dmso_aleve_
nf
RT:0.04 - 11.92
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5Time (min)
6500
7000
7500
8000
8500
9000
9500
10000
10500
56505700575058005850590059506000605061006150620062506300635064006450
Cou
nts
10.68
10.893.03
3.45 11.752.62 11.471.44 10.339.889.769.138.705.35 8.207.725.40 6.76 7.371.76 4.974.50 6.506.153.884.160.230.210.77 2.031.14 2.07
10.46
2.04
10.682.62 3.04
0.340.590.87 1.451.77 3.45 4.964.02 5.022.24 4.49 5.725.936.08 10.896.54 8.196.937.307.50 8.23 9.12 11.639.62 10.29
NL:6.46E3Channel 2 Analog 2 81315_water_ibruprofen_1
NL:1.09E4Channel 2 Analog 2 81415_dmso_ibuprofen_nf
Acetaminophen
RT:0.04 - 11.90
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5Time (min)
5800
6000
6200
6400
6600
6800
7000
7200
7400
7600
56505700575058005850590059506000605061006150620062506300635064006450
Cou
nts
10.68
10.893.04
3.46 11.7711.419.121.45 10.2910.238.93 9.831.78 8.708.198.125.36 7.474.10 4.594.88 5.88 7.436.613.90 6.532.962.060.33 0.94 2.12
2.05
10.48
10.68
3.053.3310.90 11.633.451.45 11.411.76 10.298.200.35 0.88 3.56 9.12 10.099.648.715.41 7.584.96 8.144.674.41 5.74 6.812.95 6.046.272.34 7.38
NL:6.49E3Channel 2 Analog 2 81315_water_aspirin_1
NL:7.68E3Channel 2 Analog 2 81415_dmso_aspirin_filtered_1
Aspirin
Aleve Ibuprofen
Most of the peaks are common to all the tablets, but the peak at 8.40 minutes was observed for Aleve only.
Water extract top panel
Water/DMSO extract bottom panel
Water extract top panel
Water/DMSO extract bottom panel
Figure 9. Impurity Peak in Aleve Medication
HS_MS_Aleve_1 # 129 RT: 3.71 AV: 1 SB: 43 3.22-3.54 , 3.83-4.21 NL: 1.20E5T: + c EI Q3MS [35.000-500.000]
40 60 80 100 120 140 160 180m/z
0
10
20
30
40
50
60
70
80
90
100
Rel
ativ
e A
bund
ance
91.09
92.14
65.1839.10
63.14
51.0977.20
89.0362.15 66.2645.90 78.22 107.1593.2274.2055.12 177.22 193.07152.56 163.52121.63 138.13
The peak at 8.40 min was only observed in Aleve solution.The sample was run in GC-MS to identify and the library search data showed similarity with toluene.
RT: 0.20 - 24.38
2 4 6 8 10 12 14 16 18 20 22 24Time (min)
5000
5200
5400
5600
5800
6000
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Cou
nts
10.68
8.4019.36 23.8622.5821.6618.3616.3516.00
15.123.0413.0012.401.77
3.43 10.900.24 8.184.42 4.98 5.45 10.29
NL:1.57E4Channel 2 Analog 2 81415_DMSO_Aleve_NF
8 9
ConclusionsResults and Discussion
Figure 10. Aleve Peak Confirmation by Standard • The new Fisher Chemical headspace grade solvents included in our study are all highly purified
• No extraneous peaks are observed when the blank solvents were analyzed by GC-FID-HS
• All five solvents provided an interference free base line and are suitable for trace analyte detection
• HSGC analysis of pain medications demonstrated clearly that detection of parts per billion level impuritypeak could be accomplished using these headspace solvents
RT: 2.19 - 6.23
2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4 5.6 5.8 6.0 6.2Time (min)
0
1
2
3
4
5
6
7
8
9
10
11
12
0
1
2
3
4
5
6
7
8
9
10
11
12
3.80 4.965.02
5.253.34 5.36 5.503.412.59 5.532.25 2.30 6.175.862.66 2.84 5.982.93 4.05 4.343.03 3.64 4.14
4.90 4.963.83 5.11 5.26 5.45 5.542.572.20 5.862.35 2.62 2.81 3.32 4.12 4.382.88 3.24 3.59 5.99 6.18
NL:2.47E8TIC MS 1ppm_toluene
NL:4.78E8TIC MS Aleve
figure 10
Toluene standard peak and the unknown peak in Aleve showed same retention time in GC-FID and GC-MS. GC-MS spectra from both peaks are observed identical. This confirmed the presence of toluene. The amount of toluene in Aleve medication is less than 1 ppb, which is much lower than the USP concentration limit (890 ppm).
GC-FID GC-MS
1 ppm Toluene
Aleve solution
RT: 5.24 - 9.25 SM: 15G
5.4 5.6 5.8 6.0 6.2 6.4 6.6 6.8 7.0 7.2 7.4 7.6 7.8 8.0 8.2 8.4 8.6 8.8 9.0 9.2Time (min)
55455550555555605565557055755580558555905595560056055610
10000
20000
30000
40000
50000
60000
70000
80000
90000
Cou
nts
8.29
8.985.44 8.588.175.51 7.997.22 8.677.917.46 7.565.65 7.13 9.056.865.83 6.786.556.436.316.058.30 8.31
5.485.46
5.51
5.57
5.658.075.68
5.725.745.77 7.545.82 7.64 8.025.87 7.506.45 7.04 8.63 8.667.797.266.99 8.006.26 6.61 6.83 7.426.11 8.40 9.158.72 8.91
NL:9.84E4Channel 2 Analog 2 1ug-mL_Tol_in_N-MP
NL:5.61E3Channel 2 Analog 2 aleve-in-water-fid
Toluene
Aleve
40 50 60 70 80 90 100 110 120 130 140m/z
10
20
30
40
50
60
70
80
90
100
10
20
30
40
50
60
70
80
90
100 91.16
92.17
65.1639.38 63.13 89.12 93.1751.1445.17 66.19 77.11 85.07 106.2256.10 123.25 129.12112.35 137.8698.07
91.14
92.16
65.1439.26 93.1589.1351.15 62.2245.20 66.14 77.16 106.1485.13 112.2695.2157.09 117.92 140.11
NL: 2.29E6Aleve#106 RT: 3.83 AV: 1 SB: 24 3.39-3.59 , 4.07-4.24 T: + c EI Q3MS [35.000-500.000]
NL: 3.06E61ppm_toluene#106 RT: 3.83 AV: 1 SB: 31 3.44-3.70 , 4.04-4.27 T: + c EI Q3MS [35.000-500.000]
10 11
4
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Headspace Grade Solvents for Trace Analysis of
Organic Volatile Chemicals