Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (5): 488-493.DOI: 10.3724/SP.J.1123.2020.12002
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LING Yun1, BI Jingbo1,2, YONG Wei1, YAO Meiyi1, ZHANG Yujia1, ZHANG Feng1,*()
Received:
2020-12-01
Online:
2021-05-08
Published:
2021-03-31
Contact:
ZHANG Feng
Supported by:
CLC Number:
LING Yun, BI Jingbo, YONG Wei, YAO Meiyi, ZHANG Yujia, ZHANG Feng. Simultaneous determination of eight additives in polyethylene food contact materials by ultrahigh-performance liquid chromatography[J]. Chinese Journal of Chromatography, 2021, 39(5): 488-493.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.12002
No. | Time/min | φ(A)/% | φ(B)/% |
---|---|---|---|
1 | 0.00 | 70.0 | 30.0 |
2 | 4.00 | 70.0 | 30.0 |
3 | 5.00 | 80.0 | 20.0 |
4 | 6.00 | 80.0 | 20.0 |
5 | 7.00 | 100.0 | 0.0 |
6 | 14.00 | 100.0 | 0.0 |
7 | 15.00 | 70.0 | 30.0 |
8 | 19.00 | 70.0 | 30.0 |
Table 1 Gradient elution for HPLC separation
No. | Time/min | φ(A)/% | φ(B)/% |
---|---|---|---|
1 | 0.00 | 70.0 | 30.0 |
2 | 4.00 | 70.0 | 30.0 |
3 | 5.00 | 80.0 | 20.0 |
4 | 6.00 | 80.0 | 20.0 |
5 | 7.00 | 100.0 | 0.0 |
6 | 14.00 | 100.0 | 0.0 |
7 | 15.00 | 70.0 | 30.0 |
8 | 19.00 | 70.0 | 30.0 |
Fig. 2 Extraction efficiencies of different solventsa. chloroform; b. acetone-chloroform (1∶1, v/v); c. acetonitrile-dichloromethane (1∶1, v/v); d. methylbenzene-dichloromethane (1∶1, v/v); e. methylbenzene.
Compound | Linear equation | R2 | LOD/% | LOQ/% |
---|---|---|---|---|
UV-9 | y=1.76×105x-1.60×103 | 0.9995 | 0.005 | 0.02 |
UV-71 | y=1.22×105x-1.28×103 | 0.9992 | 0.005 | 0.02 |
DIBP | y=2.17×105x-7.88×102 | 0.9994 | 0.005 | 0.02 |
Irganox 300 | y=2.93×105x-2.43×103 | 0.9995 | 0.005 | 0.02 |
DPP | y=2.08×105x-1.33×103 | 0.9995 | 0.005 | 0.02 |
UV-531 | y=1.01×105x-8.50×102 | 0.9991 | 0.005 | 0.02 |
Irganox 1076 | y=7.99×104x-1.36×103 | 0.9982 | 0.005 | 0.02 |
Irganox 168 | y=1.04×105x-1.54×103 | 0.9993 | 0.005 | 0.02 |
Table 2 Linear equations, linear ranges, correlation coefficients (R2), limits of detection (LODs), and limits of quantification (LOQs) of the eight compounds
Compound | Linear equation | R2 | LOD/% | LOQ/% |
---|---|---|---|---|
UV-9 | y=1.76×105x-1.60×103 | 0.9995 | 0.005 | 0.02 |
UV-71 | y=1.22×105x-1.28×103 | 0.9992 | 0.005 | 0.02 |
DIBP | y=2.17×105x-7.88×102 | 0.9994 | 0.005 | 0.02 |
Irganox 300 | y=2.93×105x-2.43×103 | 0.9995 | 0.005 | 0.02 |
DPP | y=2.08×105x-1.33×103 | 0.9995 | 0.005 | 0.02 |
UV-531 | y=1.01×105x-8.50×102 | 0.9991 | 0.005 | 0.02 |
Irganox 1076 | y=7.99×104x-1.36×103 | 0.9982 | 0.005 | 0.02 |
Irganox 168 | y=1.04×105x-1.54×103 | 0.9993 | 0.005 | 0.02 |
Compound | Spiked content/% | Average recovery/% | RSD/% |
---|---|---|---|
UV-9 | 0.05 | 94.8 | 2.09 |
UV-71 | 0.05 | 86.9 | 3.42 |
DIBP | 0.05 | 103.1 | 0.14 |
Irganox 300 | 0.05 | 103.4 | 2.74 |
DPP | 0.05 | 97.2 | 7.86 |
UV-531 | 0.05 | 107.7 | 0.39 |
Irganox 1076 | 0.05 | 105.9 | 4.94 |
Irganox 168 | 0.05 | 83.8 | 10.8 |
Table 3 Recoveries and RSDs of the eight compounds spiked at 0.05% in blank PE samples (n=6)
Compound | Spiked content/% | Average recovery/% | RSD/% |
---|---|---|---|
UV-9 | 0.05 | 94.8 | 2.09 |
UV-71 | 0.05 | 86.9 | 3.42 |
DIBP | 0.05 | 103.1 | 0.14 |
Irganox 300 | 0.05 | 103.4 | 2.74 |
DPP | 0.05 | 97.2 | 7.86 |
UV-531 | 0.05 | 107.7 | 0.39 |
Irganox 1076 | 0.05 | 105.9 | 4.94 |
Irganox 168 | 0.05 | 83.8 | 10.8 |
Compound | Spiked content/% | Average recovery/% | RSD/% |
---|---|---|---|
UV-9 | 0.05 | 88.4 | 8.42 |
0.2 | 99.8 | 4.61 | |
0.5 | 92.7 | 5.02 | |
UV-71 | 0.1 | 82.1 | 13.8 |
0.5 | 94.7 | 13.4 | |
0.9 | 90.1 | 12.9 | |
DIBP | 0.02 | 74.5 | 9.13 |
0.03 | 110.3 | 7.08 | |
0.05 | 95.4 | 4.96 | |
Irganox 300 | 0.03 | 82.3 | 10.6 |
0.05 | 83.8 | 9.76 | |
0.09 | 87.6 | 6.65 | |
DPP | 0.02 | 82.5 | 14.3 |
0.03 | 104.7 | 10.8 | |
0.05 | 94.4 | 4.68 | |
UV-531 | 0.1 | 89.5 | 9.65 |
0.5 | 102.1 | 4.92 | |
0.9 | 118.5 | 4.87 | |
Irganox 1076 | 0.1 | 80.7 | 10.2 |
0.5 | 89.3 | 8.96 | |
0.9 | 98.3 | 7.88 | |
Irganox 168 | 0.05 | 63.5 | 15.6 |
0.2 | 64.4 | 10.9 | |
0.5 | 75.6 | 12.4 |
Table 4 Recoveries and RSDs of the eight compounds at three spiked contents in PE quality control samples (n=6)
Compound | Spiked content/% | Average recovery/% | RSD/% |
---|---|---|---|
UV-9 | 0.05 | 88.4 | 8.42 |
0.2 | 99.8 | 4.61 | |
0.5 | 92.7 | 5.02 | |
UV-71 | 0.1 | 82.1 | 13.8 |
0.5 | 94.7 | 13.4 | |
0.9 | 90.1 | 12.9 | |
DIBP | 0.02 | 74.5 | 9.13 |
0.03 | 110.3 | 7.08 | |
0.05 | 95.4 | 4.96 | |
Irganox 300 | 0.03 | 82.3 | 10.6 |
0.05 | 83.8 | 9.76 | |
0.09 | 87.6 | 6.65 | |
DPP | 0.02 | 82.5 | 14.3 |
0.03 | 104.7 | 10.8 | |
0.05 | 94.4 | 4.68 | |
UV-531 | 0.1 | 89.5 | 9.65 |
0.5 | 102.1 | 4.92 | |
0.9 | 118.5 | 4.87 | |
Irganox 1076 | 0.1 | 80.7 | 10.2 |
0.5 | 89.3 | 8.96 | |
0.9 | 98.3 | 7.88 | |
Irganox 168 | 0.05 | 63.5 | 15.6 |
0.2 | 64.4 | 10.9 | |
0.5 | 75.6 | 12.4 |
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