Chinese Agricultural Science Bulletin ›› 2021, Vol. 37 ›› Issue (32): 148-156.doi: 10.11924/j.issn.1000-6850.casb2020-0731
Special Issue: 水产渔业
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Yin Yuting1(), Wang Qian2,3,4, Chen Xi1,2, Gui Yuan1, Song Chao1,2,3,4(
)
Received:
2020-11-29
Revised:
2021-05-06
Online:
2021-11-15
Published:
2022-01-07
Contact:
Song Chao
E-mail:1669881749@qq.com;songc@ffrc.cn
CLC Number:
Yin Yuting, Wang Qian, Chen Xi, Gui Yuan, Song Chao. Determination of Residual Arsenic in the Chinese Mitten Crabs (Eriocheir sinensis) by HPLC-ICP-MS[J]. Chinese Agricultural Science Bulletin, 2021, 37(32): 148-156.
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URL: https://www.casb.org.cn/EN/10.11924/j.issn.1000-6850.casb2020-0731
参数名称 | 参数(HPLC-ICP-MS) |
---|---|
雾化室 | 2℃ |
采样深度 | 8.0 mm |
IF/BK 真空度 | 180 kPa |
反馈功率 | <10 W |
雾化器压力 | 364 kPa |
等离子体(氩气)流量 | 15.00 L/min |
辅助气流量 | 1.00 L/min |
雾化器流量 | 1.00 L/min |
补偿/稀释气流量 | 1.00 L/min |
参数名称 | 参数(HPLC-ICP-MS) |
---|---|
雾化室 | 2℃ |
采样深度 | 8.0 mm |
IF/BK 真空度 | 180 kPa |
反馈功率 | <10 W |
雾化器压力 | 364 kPa |
等离子体(氩气)流量 | 15.00 L/min |
辅助气流量 | 1.00 L/min |
雾化器流量 | 1.00 L/min |
补偿/稀释气流量 | 1.00 L/min |
序号 | 流动相A | 流动相B | 流动相成分组成/% | 流速/(mL/min) |
---|---|---|---|---|
1 | 10 mM/L无水乙酸钠、3 mM/L硝酸钾、10 mM/L磷酸二氢钠、 0.2 mM/L乙二胺四乙酸二钠(pH 8.4) | 无水乙醇(C2H6O) | 99%+1% | 1.0 |
2 | 25 mM/L NH4H2PO4(pH 8.0) | 水 | 75%+25% | 1.0 |
3 | 10 mM/L (NH4)2HPO3(pH 8.0) | 水 | 100% | 1.0 |
4 | 50 mM/L (NH4)2CO3(pH 10.0) | 水 | 100% | 1.0 |
序号 | 流动相A | 流动相B | 流动相成分组成/% | 流速/(mL/min) |
---|---|---|---|---|
1 | 10 mM/L无水乙酸钠、3 mM/L硝酸钾、10 mM/L磷酸二氢钠、 0.2 mM/L乙二胺四乙酸二钠(pH 8.4) | 无水乙醇(C2H6O) | 99%+1% | 1.0 |
2 | 25 mM/L NH4H2PO4(pH 8.0) | 水 | 75%+25% | 1.0 |
3 | 10 mM/L (NH4)2HPO3(pH 8.0) | 水 | 100% | 1.0 |
4 | 50 mM/L (NH4)2CO3(pH 10.0) | 水 | 100% | 1.0 |
砷形态 | 线性范围/(μg/L) | 线性方程 | 相关系数 | 检测限/(μg/kg) | 定量限/(μg/kg) |
---|---|---|---|---|---|
AsC | 0-50 | y=3209.8435x-899.2297 | 0.9990 | 0.015 | 0.05 |
AsB | 0-50 | y=2744.3x-197.09 | 0.9995 | 0.0912 | 0.304 |
As(Ⅲ) | 0-50 | y=12167x +3.4427 | 0.9999 | 0.006 | 0.02 |
DMA | 0-50 | y=2966.3x +8.9858 | 0.9998 | 0.006 | 0.02 |
MMA | 0-50 | y=2817.1x-37.093 | 0.9999 | 0.015 | 0.05 |
As(V) | 0-50 | y=14525x +221.65 | 0.9997 | 0.0159 | 0.053 |
砷形态 | 线性范围/(μg/L) | 线性方程 | 相关系数 | 检测限/(μg/kg) | 定量限/(μg/kg) |
---|---|---|---|---|---|
AsC | 0-50 | y=3209.8435x-899.2297 | 0.9990 | 0.015 | 0.05 |
AsB | 0-50 | y=2744.3x-197.09 | 0.9995 | 0.0912 | 0.304 |
As(Ⅲ) | 0-50 | y=12167x +3.4427 | 0.9999 | 0.006 | 0.02 |
DMA | 0-50 | y=2966.3x +8.9858 | 0.9998 | 0.006 | 0.02 |
MMA | 0-50 | y=2817.1x-37.093 | 0.9999 | 0.015 | 0.05 |
As(V) | 0-50 | y=14525x +221.65 | 0.9997 | 0.0159 | 0.053 |
砷形态 | 加标浓度/(μg/kg) | 回收率/% | RSD/% | |||||
---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 1 | 2 | 3 | |||
AsC | 0.5 | 5 | 50 | 77.052 | 82.917 | 93.285 | <5% | |
AsB | 0.5 | 5 | 50 | 76.177 | 119.949 | 109.888 | <5% | |
As(Ⅲ) | 0.5 | 5 | 50 | 71.981 | 80.317 | 74.501 | <5% | |
DMA | 0.5 | 5 | 50 | 100.093 | 87.779 | 94.670 | <5% | |
MMA | 0.5 | 5 | 50 | 99.933 | 84.800 | 88.777 | <5% | |
As(V) | 0.5 | 5 | 50 | 71.654 | 76.655 | 74.083 | <5% |
砷形态 | 加标浓度/(μg/kg) | 回收率/% | RSD/% | |||||
---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 1 | 2 | 3 | |||
AsC | 0.5 | 5 | 50 | 77.052 | 82.917 | 93.285 | <5% | |
AsB | 0.5 | 5 | 50 | 76.177 | 119.949 | 109.888 | <5% | |
As(Ⅲ) | 0.5 | 5 | 50 | 71.981 | 80.317 | 74.501 | <5% | |
DMA | 0.5 | 5 | 50 | 100.093 | 87.779 | 94.670 | <5% | |
MMA | 0.5 | 5 | 50 | 99.933 | 84.800 | 88.777 | <5% | |
As(V) | 0.5 | 5 | 50 | 71.654 | 76.655 | 74.083 | <5% |
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