»
SEPARATIONS AND PURIFICATIONS
» Table 7. Repeatability of 1 µg/mL (ppm) Standard Concentration on Secondary Wavelength
Element Concentration 1 µg/mL (ppm) Mg
Element Wavelength (nm).
Prep 1, Run 1 Prep 1, Run 2 Prep1, Run 3 Mean
Std. Dev. %RSD
Prep 2, Run 1 Prep 2, Run 2 Prep2, Run 3 Mean
Std. Dev. %RSD
Prep 3, Run 1 Prep 3, Run 2 Prep3, Run 3 Mean
Std. Dev. %RSD
Overall Average Overall Std. Dev Overall %RSD
Al
285.213 1.021 1.084 1.043 1.029
0.0123 1.19
0.983 0.988 0.991 0.987
0.0043 0.44
0.981 0.982 1.033 0.999
0.0298 2.98
1.005 0.025 2.47
396.153 0.989 1.044 1.018 1.020
0.0152 1.49
0.976 0.964 1.010 0.983
0.0238 2.42
1.014 0.976 1.012 1.001
0.0213 2.13
1.001 0.024 2.37
Sn
235.485 1.012 1.063 1.096 1.086
0.0088 0.81
1.035 1.046 1.048 1.043
0.0071 0.68
1.031 1.033 1.080 1.048
0.0276 2.63
1.059 0.025 2.40
Os
228.226 1.001 1.038 1.071 1.062
0.0081 0.76
1.011 1.018 1.018 1.016
0.0036 0.35
1.008 1.009 1.052 1.023
0.0252 2.46
1.033 0.025 2.44
Rh
343.489 1.010 1.066 1.047 1.034
0.0122 1.18
0.983 0.991 0.998 0.991
0.0077 0.78
0.976 0.987 1.026 0.996
0.0259 2.60
1.007 0.025 2.52
Ir
224.268 1.000 1.023 1.018 1.020
0.0062 0.61
0.965 0.976 0.977 0.973
0.0070 0.72
0.955 0.973 1.005 0.978
0.0252 2.58
0.990 0.026 2.65
Pd
340.458 1.041 1.098 0.876 0.871
0.0053 0.61
0.838 0.846 0.847 0.844
0.0051 0.60
0.845 0.847 0.879 0.857
0.0187 2.19
0.876 0.064 7.30
Ni
232.003 1.022 1.070 1.041 1.031
0.0100 0.97
0.992 0.991 0.997 0.993
0.0034 0.34
0.992 0.983 1.030 1.001
0.0251 2.50
1.007 0.020 1.96
Timepoint (Days)
0 1 4 6 8
Mean %RSD
Timepoint (Days) Ni
0 1 4 6 8
Mean %RSD
232.003 98.0
103.0 103.3 106.6 101.2
Cu
327.393 99.5
101.8 99.6
105.0 102.3
2.2
Table 8. Stability on Standard Solution Stored Over 8 Days at Room Temperature Condition: Ambient (Room Temperature)
Ni
231.604 99.2
103.1 102.9 105.9 101.5
Cu
324.752 99.5
101.4 99.1
105.0 101.8
2.4 Zn
206.200 99.9
104.7 104.5 106.4 104.0
1.0 Fe
238.204 98.3
103.4 102.0 105.4 105.3
1.6 Mg
285.213 101.5 101.8 99.5
105.0 101.0
2.3 Sn
235.485 96.2
104.4 103.1 105.6 102.5
1.3 Pd
340.458 94.4
106.3 104.7 106.0 96.7
4.4 Pt
265.945 98.4
103.3 103.6 105.9 98.9
2.8 Ru
240.272 96.8
103.4 103.1 106.2 100.4
103.4 101.8 104.9 104.0 101.8 103.9 103.4 102.9 103.3 1.8
2.3
Condition: Ambient (Room Temperature) Zn
Fe
213.857 100.3 104.4 103.6 105.6 103.4
1.0
239.562 99.5
102.5 101.2 104.8 104.8
1.7 Mg
279.077 98.5
103.4 103.9 106.1 102.0
1.6 Sn
283.998 95.5
104.1 104.0 106.0 100.6
2.2 Pd
363.470 87.4
113.4 109.6 111.1 101.0
5.0 Pt
214.423 98.6
103.2 103.2 106.3 98.0
3.4 Ru
349.894 96.0
102.8 103.5 106.7 100.2
103.5 102.2 104.3 103.3 103.9 103.7 108.8 102.7 103.3 2.2
2.6
(at nominal concentration, stored at room temperature and at refrigerated conditions
42 | | January/February 2015
[2°C to 8°C]) were evaluated against a freshly prepared standard mixture over an extended
Conclusion
A generic ICP-OES method was successfully developed, optimized, and validated for trace metal analysis of 9 elements commonly used in the pharmaceutical industry. The method is suitable for projects in the early stages of development and could be extended to late stage/commercial products with minimal additional work by evaluating the robustness
period of time. The samples were tested on Days 0, 1, 4, 6, and 8 with ICP-OES and the results are summarized in Tables 8 and 9. The percent recoveries of standard solutions stored at room temperature and refrigerated conditions were within 80 to 120% with %RSD <5. The standard solutions are stable for at least 8 days (192 hours) under both storage conditions. The validation of the method demonstrated the standard solution is stable during the whole analytical procedure before and after analysis.
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