Determination of 16 sulfonamide residues in livestock and poultry meat. Liquid chromatography-tandem mass spectrometry (2)

2.
2.
3.
6 Determination

(1) Liquid chromatography conditions

Column: Lichrospher 100RP-18, 5um, 250mm×4.
6mmi.
d.
or equivalent; mobile phase: acetonitrile + 0.
01 mol/L ammonium acetate solution (12+88, v/v); flow rate: 0.
8mL/min; Column temperature: 35°C; injection volume: 40μL; split ratio: 1:3
.

(2) Mass spectrometry conditions

Ion source: electrospray ion source; scanning method: positive ion scan; detection method: multi-reaction monitoring; electrospray voltage: 5500V; atomizing gas pressure: 0.
076MPa; curtain air pressure: 0.
069MPa; auxiliary gas flow rate: 6L/min ; Ion source temperature: 350℃; qualitative ion pair, quantitative ion pair, collision gas energy and declustering voltage are shown in Table 2-15
.

Table 2-15 Qualitative ion pairs, quantitative ion pairs, collision gas energy and declustering voltage of 16 sulfonamides

(3) Liquid chromatography-tandem mass spectrometry determination

Samples were injected separately with mixed standard working solutions, with the concentration of the working solution (ng/mL) as the abscissa and the peak area as the ordinate, draw a standard working curve, use the standard working curve to quantify the sample, and the response of 16 sulfonamides in the sample solution The values ​​should be within the linear range measured by the instrument
.

Figure 2-4 Total ion current diagram of 5 kinds of sulfonamide mixed standard materials