邹耀华,王红青,潘佳星.QuEChERS-UPLC-MS/MS法测定龟甲中孔雀石绿和隐性孔雀石绿残留量[J].中国药品标准,2018,19(5):342-345 |
QuEChERS-UPLC-MS/MS法测定龟甲中孔雀石绿和隐性孔雀石绿残留量 |
Determination of malachite green and leucomalachite green in tortoise shell by QuEChERS-UPLC-MS/MS |
投稿时间:2018-06-30 修订日期:2018-09-27 |
DOI: |
中文关键词: UPLC-MS/MS 龟甲 孔雀石绿 隐性孔雀石绿 |
英文关键词: UPLC-MS/MS tortoise shell malachite green leucomalachite green |
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中文摘要: |
目的:建立超高效液相色谱-串联三重四极杆质谱法快速测定龟甲中孔雀石绿和隐性孔雀石绿残留量的检测方法。方法:样品采用5%甲酸乙腈溶液提取,用二异氰酸酯多元醇共聚物(EMR)净化,采用C18色谱柱分离,以5mmol/L醋酸铵溶液和乙腈梯度洗脱,采用选择离子监测(Target MS/MS)模式检测。结果:孔雀石绿在0.096μg/L~2.4μg/L范围内线性良好(r=0.9989),三个浓度加标回收率为90.8~103.3%(n=9);隐性孔雀石绿在0.087μg/L~2.18μg/L范围内线性良好(r=0.9994),三个浓度加标回收率为67.1~83.8%(n=9),多批次样品中检测出孔雀石绿和隐性孔雀石绿。结论:本方法可以用于快速测定龟甲中孔雀石绿和隐性孔雀石绿残留量。 |
英文摘要: |
Objective: To establish a method for rapid determination of the residues of malachite green and leucomalachite green in tortoise shell by UPLC-MS/MS. Methods: Samples were extracted with 5% formic acid and acetonitrile solution, purified by diisocyanate polyol copolymer (EMR), separated by C18 column, gradient elution with 5mmol/L ammonium acetate solution and acetonitrile, and detected by selective ion monitoring (Target MS/MS) mode. Results: Good linearity of malachite green in 0.096 µg/L ~2.4 µg/L range of three concentration(r=0.9989), the recoveries were 90.8 ~ 103.3% (n=9); good linearity of leucomalachite green in 0.087 µg/L~2.18 µg/L range of three concentration(r=0.9994),the recoveries were 67.1 ~ 83.8% (n=9); multiple batches of samples were be detected malachite green and Leucomalachite green. Conclusion: This method can be used for rapid determination of malachite green and leucomalachite green in tortoise shell. |
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