Determination method of catalin content in rat plasma after oral administration of Duyiwei
A technology of flax glycosides and a determination method, which is applied in the fields of medical detection and in vivo metabolism research of Chinese patent medicines, can solve the problems of difficult cracking to form daughter ions, inability to detect the content of flax glycosides, etc., and achieves accurate, reliable and reproducible determination results. Excellent, high-precision results
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Embodiment 1
[0060] Example 1 Determination of the content of catalin components in rat plasma after oral administration of Duyiwei whole herb and ground medicinal materials
[0061] Include the following steps:
[0062] 1.1 Preparation of plasma test samples:
[0063] (1) Dissolve the extract of the aerial part of Duyiwei in an appropriate amount of 0.5% CMC-Na solution to obtain a 50 mg / mL solution, and give 0.8 g / kg of the Duyiwei solution to rats (250 ± 20 g) by intragastric administration;
[0064] (2) 0.3 mL of blood was collected from the orbit of the rat at 5 min, 15 min, 0.5 h, 1 h, 1.5 h, 2 h, 3 h, 4 h, 6 h, 8 h, 12 h and 24 h after administration, and placed in 1.5 mL of heparinized polymer Immediately centrifuge at a constant temperature of 4°C for 10 minutes at a constant temperature of 4000×g in an ethylene tube to obtain plasma;
[0065] (3) Take 0.1mL plasma and place it in a 1.5mL EP tube, add 0.3mL methanol solution (containing 0.1% formic acid and 200ng / mL tinidazole i...
Embodiment 2
[0076] The optimization of embodiment 2 detection conditions
[0077] 2.1 Optimization of mass spectrometry conditions
[0078] Taking the catalin standard solution as the object, the mass spectrometry detection conditions were determined by adjusting the fragmentation voltage and the collision voltage, and the mass spectrometry conditions were finally determined as shown in Table 1.
[0079] Table 1 Optimized the collision energy required for the formation of stable ions by catalin and tinidazole reference substances in MRM mode
[0080]
[0081]
[0082] 2.2 Optimization of chromatographic conditions
[0083] (1) The separation conditions of similar substances in the reference literature are determined to add 0.1% formic acid to adjust the acidity. Afterwards, the two mobile phase compositions of acetonitrile-water (containing 0.1% formic acid) and methanol-water (containing 0.1% formic acid) are investigated respectively, and the results are shown in Figure 2-3 , ...
Embodiment 3
[0088] Embodiment 3 Methodology Verification Experiment 2
[0089] 3.1 Examination of specificity
[0090] The rat plasma after oral administration of the aerial parts of Duyiwei, the blank plasma solution with the addition of the standard product of cataside and the blank plasma solution without the standard product of cataside were operated according to the above-mentioned extraction conditions, and were detected according to the above-mentioned chromatographic mass spectrometry conditions. For comparison, see the results Figure 20-22 . It can be seen from the figure that the detection method has good specificity and can meet the detection requirements.
[0091] 3.2 Investigation of linear relationship
[0092] With 7 different concentrations of cataside solutions, operate according to the above-mentioned extraction conditions, measure according to the above-mentioned chromatographic mass spectrometry conditions, and use the concentration as the abscissa, and the peak ar...
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