Selection of Analysis Conditions for Determination of Zearalenol Residues in Food of Animal Origin

9.

(1) Selection of chromatographic separation conditions

A reversed-phase C ₁₈ column was used for separation, acetonitrile -water was used as the mobile phase, and gradient elution was used.

(2) Selection of mass spectrometry conditions

Tandem mass spectrometry adopts MRM mode detection, β-zearalenol : select ion pairs m/z321.

(3) Qualitative and quantitative methods.

When performing sample determination, if the deviation between the retention time of the detected chromatographic peak and the retention time of the standard is within ±2.

9.

When the external standard method is used for quantification, in order to eliminate the influence of the matrix on the detection, the matrix standard solution that is the same or similar to the sample to be tested is usually used for calibration

According to the recovery test, the lowest concentration that can be quantitatively measured is the lower limit of determination (LOQ, S/N>10), and the LOQ is 1μg/kg, which meets the detection requirements of the highest limit (1μg/kg)

9.

Take an appropriate amount of standard substance and add it to the 5g blank sample to make the addition amount equivalent to 1μg/kg, 2μg/kg, 5μg/kg and 10μg/kg, carry out sample processing and determination, and use the external standard method to calculate the recovery rate

9.

Under the repeatability test conditions, the absolute difference between the two independent test results obtained does not exceed the repeatability limit r, the concentration range and repetition of β-zearalenol, zearalenol and zearalenone in the sample The sex equation is shown in Table 9-31

Table 9-30 Method recovery and precision (n=10)

Table 9-31 Content range and repeatability and reproducibility equation