A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry
A technology of high performance liquid chromatography and prohexidine hydrochloride, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of high accuracy and precision, low detection limit, and easy operation
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Embodiment 1
[0026] Example 1 Method optimization for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry
[0027] 1. Optimization of mass spectrometry conditions
[0028] Inject 10 mg / L of chlorhexenidine hydrochloride, chlorhexidine hydrochloride-d8, p-chlorobenzamide acetic acid, and p-chlorobenzoic acid into the mass spectrometer through a syringe pump, and the responses of the above-mentioned target substances in positive ion and negative ion modes The results showed that the responsivity of chlorhexidine hydrochloride and chlorhexidine-d8 in positive ion mode was 5 times and 3 times that in negative ion mode. However, the response values of p-chlorobenzamide acetic acid and p-chlorobenzoic acid in the negative ion mode were 2 times and 1 times that in the positive ion mode. Therefore, chlorhexidine hydrochloride and chlorhexidine-d 8 The analysis was performed in positive...
Embodiment 2
[0037] A method for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products based on high performance liquid chromatography-tandem mass spectrometry of time-segmented technology, the steps are:
[0038] A. Weigh 1g of homogeneous grass carp muscle sample in a 15mL centrifuge tube, add chlorhexenidine hydrochloride, p-chlorobenzamide acetic acid and p-chlorobenzoic acid standard solution to make chlorhexenidine hydrochloride, p-chlorobenzamide The concentrations of acetic acid and p-chlorobenzoic acid were 1, 3, 50, 100, 400 μg / kg, 2.5, 5, 50, 100, 400 μg / kg, 5, 10, 50, 50 μg / kg, and then 20 μL of 1 mg / kg L Chlorhexidine Hydrochloride-d 8 Internal standard solution, shake for 30s, add 5mL extractant acetonitrile containing 1% formic acid, shake for 30s, ultrasonically extract for 5min, add 1g of anhydrous magnesium sulfate to remove water and part of fat in the sample, vortex. Centrifuge at 8000r / min for 5min, put the upper liquid in anot...
Embodiment 3
[0056] Application of time-segmented high performance liquid chromatography-tandem mass spectrometry for the determination of prohezidine hydrochloride and its metabolite residues in aquatic products:
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