The linear range and detection limit of 14 quinolones residues in honey

11.
2.
2.
8 Linearity range and lower detection limit

The quinolone sensitive drugs, dubbed a series of sample blank solution matrix standard working solution, measured at selected chromatographic conditions and mass spectrometry conditions, 40 L injection volume, the substrate for the working standard solution is measured by peak area group Plot the concentration of the components, and the linear range, linear equation and linear correlation coefficient are shown in Table 11-15
.

Table 11-15 The linear ranges, linear equations and correlation coefficients of the fourteen quinolone drugs

Thus, in the process operating conditions, ciprofloxacin 0.
4 ~ 100.
0ug / kg, oxolinic acid in 0.
4 ~ 50.
0μg / kg, enrofloxacin , sarafloxacin , difloxacin , enoxaparin gatifloxacin , norfloxacin in 1.
0 ~ 100.
0μg / kg, ofloxacin , danofloxacin , fleroxacin , orbifloxacin , marbofloxacin at 1.
0 ~ 50.
0μg / kg, 2.
0 ~ flumequine Within the concentration range of 100.
0μg/kg, the response values ​​are all within the linear range of the instrument
.
The signal-to-noise ratio of each quinolone peak height is greater than 5 to determine the minimum detection limit of the method

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2.
2.
9 Method recovery and precision

Use honey samples without quinolones to carry out addition recovery and precision experiments.
After adding different concentration standards to the samples, leave them for 1 hour to make the standards fully absorbed by the sample, and then extract and purify according to this method, using liquid chromatography-tandem For quadrupole mass spectrometry, the recovery and precision results are shown in Table 11-16
.
It can be seen from Table 11-16 that this method has four addition levels of 2.

Table 11-16 Addition recovery rate (%) and precision of quinolone in honey

Table 11-17 Experimental data of the recovery rate of quinolones in different honey species

11.
2.
2.

Under repeatability test conditions, the absolute difference between the two independent test results obtained does not exceed the repeatability limit (r).

Table 11-18 Content range and repeatability and reproducibility equation