A method for separating or analyzing phenolic compounds from burdock
A technology for phenolic acids and compounds, applied in the field of active ingredient separation, can solve the problems of unstable and time-consuming derivatization of phenolic acid substances, and achieve the effects of improving duty cycle and sensitivity, large peak capacity, and stable derivatization.
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Embodiment 1
[0081] (1) Preparation of the test solution:
[0082] The burdock leaves were sliced and dried into dry powder, then refluxed with 70% ethanol to extract for 3 hours, then added 0.15% of the total volume of hydrochloric acid to extract twice, mixed and concentrated under reduced pressure at 40°C, and then frozen Dry, add volume concentration and be mixed with the chromatographic methanol of 80% need testing solution;
[0083] (2) Prepare standard stock solution by reference product:
[0084] Weigh 3,4-dihydroxybenzoic acid, 2,5-dihydroxybenzoic acid, trans-p-coumaric acid, quimaric acid, vanillic acid, caffeic acid, trans-ferulic acid, sinapinic acid, all with volume concentration 80% chromatographic methanol is prepared as a standard stock solution with a substance concentration of 100ppm;
[0085] (3) Preparation of mixed standard solution:
[0086] Accurately measure the standard stock solution of 8 kinds of phenolic acid compounds, use described 80% chromatographic me...
Embodiment 2
[0090] Adopt the operation process as embodiment 1, wherein:
[0091] The chromatographic conditions of high performance liquid chromatography are as follows:
[0092] The size is 2.1mm×100mm, 3.0μm C18 column, the mobile phase is composed of mobile phase A and mobile phase B, wherein mobile phase A is an aqueous solution containing 0.1% formic acid, mobile phase B is methanol or acetonitrile, and the gradient is carried out under the following conditions Elution: 0~0.05min, 5%~35% mobile phase B; 0.05~15min, 35%~55% mobile phase B; 15~25min, 55%~100% mobile phase B; volume flow rate is 0.15mL. min -1 ; The injection volume is 5 μL; min -1 ; Ion mobility spectrometry conditions are as follows:
[0093]
[0094]
[0095] The signal-to-noise ratio of the obtained ion mobility spectrum was analyzed to obtain the following figure 1 In the statistical results shown, in each group of columns in the figure, the column on the left is acetonitrile, and the column on the righ...
Embodiment 3
[0097] Use the operation process as embodiment 1, wherein:
[0098] The chromatographic conditions of the high-performance liquid chromatography are as follows: the specification is 2.1mm×100mm, 3.0μm C18 column, the mobile phase is composed of mobile phase A and mobile phase B, wherein mobile phase A is 0.1% formic acid aqueous solution or 0.1% acetic acid aqueous solution , the mobile phase B is methanol, and the following conditions are used for gradient elution: 0-0.05min, 5%-35% mobile phase B; 0.05-15min, 35%-55% mobile phase B; 15-25min, 55%-100 % mobile phase B; the volume flow rate is 0.15mL. min -1 ; The injection volume is 5 μL; the column temperature is 35°C; post-column replenishment is preferred, and the flow rate of the post-column replenishment solution is 0.1mL. min -1 ;
[0099] The ion mobility spectrometry conditions are as follows:
[0100]
[0101]
[0102] The signal-to-noise ratio of the obtained ion mobility spectrum was analyzed to obtain t...
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