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Introduce the rapid determination method of liquid chromatography-tandem mass spectrometry (according to GB/T19857-2005)
.
1.
Principle
The residue in the sample is extracted with acetonitrile - ammonium acetate buffer solution.
After acetonitrile is extracted again, the liquid is distributed to the methylene chloride layer, purified by neutral alumina and cationic solid phase column, and then determined by liquid chromatography-tandem mass spectrometry.
, Quantification by internal standard method
.
The residual amount of malachite green, leuco malachite green, crystal violet and leuco crystal violet in the sample is calculated as follows (the blank value needs to be deducted from the calculation result):
Where X——the residual amount of the component to be tested in the sample, ug/kg
p——The concentration of the standard working solution of malachite green, leuco malachite green, crystal violet or leuco crystal violet, ug/L
p si ——concentration of internal standard substance in standard working solution, ug/L
p i ——concentration of internal standard substance in sample solution, pg/L
A s ——The peak area of the standard working solution of malachite green, leuco malachite green, crystal violet or leuco crystal violet
A——The peak area of malachite green, leuco malachite green, crystal violet or leuco crystal violet in the sample solution
A si —The peak area of the internal standard substance in the standard working solution
A i ——The peak area of the internal standard substance in the sample solution
V——Constant volume of sample, mL
m——sample weight, g
2.
Liquid chromatography-tandem mass spectrometry conditions
Chromatographic column: C18 column, 50mm×2.
Atomizing gas, curtain gas, auxiliary heating gas, and collision gas are all high-purity nitrogen.
The spray voltage, declustering voltage, collision energy and other voltage values should be optimized to the optimal sensitivity
Monitoring ion pair: malachite green m/z329/313 (quantitative ion), 329/208; leuco malachite green m/z331/316 (quantitative ion), 331/239; crystal violet m/z372/356 (quantitative ion) ), 372/251; leuco crystal violet m/z374/359 (quantitative ion), 374/238; fluorinated malachite green m/z334/318 (quantitative ion); fluorinated leuco malachite green m/z337/ 322 (quantitative ion)
3.
(1) This method is suitable for the detection of the residual amount of malachite green and its metabolite leuco malachite green, crystal violet and its metabolite leuco crystal violet in fresh aquatic products and their products
(2) The result of the determination of the residual amount of malachite green in this method refers to the sum of the residual amount of malachite green and its metabolite leucomalachite green, expressed as malachite green; the result of the determination of the residual amount of crystal violet refers to crystal violet And its metabolite leuco crystal violet residual amount, expressed as crystal violet
(3) The detection limit of the method: the detection limits of malachite green, leuco malachite green, crystal violet, and leuco crystal violet are all 0.
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