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1.
6 Determination
(1) Liquid chromatography conditions
Chromatographic column: Atlantis, 3um, 150mm×2.
1mm (inner diameter) or equivalent; mobile phase: A is acetonitrile , B is 0.
1% formic acid solution, and C is methanol
.
See Table 2-5 for gradient elution conditions; flow rate: 0.
Table 2-5 Mobile phase gradient conditions
(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 2-6
.
Table 2-6 Qualitative ion pairs, quantitative ion pairs, collision gas energy and declustering voltage of 18 sulfonamides
(3) Liquid chromatography-tandem mass spectrometry determination
Samples were injected separately with the matrix mixed standard working solution, and the ratio of the peak area of each standard to the peak area of the internal standard was used as the ordinate, and the ratio of the concentration of each standard working solution to the concentration of the internal standard solution was used as the abscissa to draw the standard working curve.
The working curve quantifies the sample, and the response values of the 18 sulfonamides in the sample solution should all be within the linear range determined by the instrument
Figure 2-1 Multiple reaction monitoring (MRM) chromatograms of 18 sulfonamide reference materials
Related links: Determination of 18 sulfonamide residues in puffer fish and eels by liquid chromatography-tandem mass spectrometry (1)