In order to effectively extract chlorogenic acid and explore the zui optimization process conditions for extracting chlorogenic acid from wild chrysanthemum, the authors used orthogonal experiments to investigate the extraction process of chlorogenic acid from wild chrysanthemum by two methods: water bath extraction and ultrasonic assisted extraction. Orthogonal optimization, in order to find the preparation process of Zui Jia.
1 instruments and materials 1.1 instrument UV / VIS916 spectrophotometer (Australia GBC), ZK-82A vacuum drying oven (Shanghai Laboratory Instrument Factory), FZ102 micro-plant sample crusher (Hebei Province Huanghua City Zhenxing Electromechanical Instrument Factory ), SX8200H desktop ultrasonic cleaner (Shanghai Branch Guide Ultrasonic Instrument Co., Ltd.), HH-S2 series constant temperature water bath (Jintan Huanyu Scientific Instrument Factory, Jiangsu Province).
1.2 Materials The chlorogenic acid standard was purchased from the China National Institute for the Control of Pharmaceutical Biology. The wild chrysanthemum was purchased from Bangjian Pharmacy (baked at 50 ° C for 3 h, pulverized for use), and other reagents were of analytical grade.
2 Methods and Results 2.1 Preparation of reference solution Accurately weigh 5.2mg of chlorogenic acid reference substance in a 250ml volumetric flask, dissolve it with 70% ethanol solution, and obtain the volume.
2.2 Determination of the measurement wavelength Take 1ml of the reference solution, placed in a 10ml volumetric flask, and made up to 70% ethanol. The 70% ethanol solution was used as a reference solution, and the large absorption wavelength of zui was scanned on a UV spectrophotometer in the range of 200 to 400 nm. As a result, there was a large absorption peak at 329.6 nm, and 329.6 nm was selected as the measurement wavelength.
2.3 Methodology 2.3.1 Drawing of the standard curve Precision draw the reference solution 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 1.0, 2.0, 3.0, 4.0 ml in 10 10 ml volumetric flasks, and make up to 70% ethanol. The absorbance was measured at λ = 329.6 nm on an ultraviolet spectrophotometer. The absorbance A is plotted on the ordinate and the chlorogenic acid concentration C is plotted on the abscissa. A standard curve is drawn. The regression equation obtained by linear regression is: A=51.133C-0.0058, r=0.9997. The results show that chlorogenic acid has a good linear relationship in the range of 0.416~4.576g·L-1.
2.3.2 Precision test Accurately weigh about 1g of wild chrysanthemum, add 10ml and extract in 70°C water bath for 60min, accurately absorb 1ml of extract, put it in 10ml volumetric flask, and make up to 70% ethanol. The absorbance was measured by using 70% ethanol as a blank. Continuous measurement 6 times, RSD = 0.72%, indicating that the instrument precision is better.
2.3.3 Stability test Accurately absorb 1 ml of the extract obtained in “2.3.2â€, place it in a 10 ml volumetric flask, and make up to 70% ethanol. The absorbance was measured at 0, 10, 20, 30, 40, 50 min with 70% ethanol as the blank, and the measurement was repeated 6 times, RSD = 0.38%, indicating that the extract was stable within 1 h.
2.3.4 Repeatability experiment Weigh accurately about 1g of wild chrysanthemum powder, and prepare 3 parts of extract according to the “2.3.2†method. According to the “2.3.2†method, RSD=0.25%, indicating the method repeatability. it is good.
2.3.5 Sample recovery rate experiment Different amounts of chlorogenic acid reference substance were added to the known content of wild chrysanthemum, and the absorbance was measured by ultraviolet spectrophotometer to obtain the chlorogenic acid content. The average recovery was 100.89%, and the RSD was 1.45%, indicating that the method recovery rate was better.
2.4 orthogonal experimental design [3,4]
2.4.1 Water bath extraction method Under the same conditions of particle size and extraction process, the factors such as water bath temperature, ethanol concentration, liquid-solid ratio and extraction time were investigated, and the experiment was arranged by L9 (34) orthogonal table. See Table 1. Table 1 water bath extraction factor level (omitted)
2.4.2 Ultrasonic extraction method Under the same conditions of particle size and extraction process, the factors such as immersion time, ethanol concentration, liquid-solid ratio and ultrasonic time were investigated. The experiment was arranged by L9 (34) orthogonal table. See Table 2. Table 2 ultrasonic method factor level (omitted)
2.5 Determination of wild chrysanthemum [5] Precision weighed about 1g of wild chrysanthemum, placed in a 100ml round bottom flask, according to the "2.4" item for orthogonal experiment, the extract was suction filtered, the filtrate was quantitatively transferred to a 100ml volumetric flask, 70% Make up to volume of ethanol. 1 ml of the filtrate was accurately aspirated in a 10 ml volumetric flask, the absorbance was measured according to the standard curve preparation method, and the chlorogenic acid content was calculated from the standard absorption curve. The results are shown in Table 3. Table 3 orthogonal experimental scheme and results analysis (omitted)
2.6 Analysis of variance According to Table 3, the extraction conditions of the water bath extraction method were as follows: A3B2C2D1, that is, 70% ethanol with a liquid-solid ratio of 12:1 was extracted in a water bath at 80 ° C for 40 min. Under this condition, the chlorogenic acid content reached 0.35%. From the range analysis, the order of influence of various factors on chlorogenic acid extraction was extraction temperature > liquid-solid ratio > ethanol concentration > extraction time.
The extraction conditions of the ultrasonic extraction method were as follows: A2B2C2D3, which was pre-impregnated with 60% ethanol with a liquid-solid ratio of 15:1 for 40 min, and ultrasonic extraction for 45 min. Under this condition, the mass fraction of chlorogenic acid reached 0.36%. From the range analysis, the order of influence of various factors on chlorogenic acid extraction was ethanol concentration>immersion time>ultrasonic time>liquid-solid ratio.
3 Conclusions The orthogonal extraction experiments confirmed that the extraction conditions of the water bath extraction method were as follows: 70% ethanol with a liquid-solid ratio of 12:1 was extracted in a water bath at 80 °C for 40 min. Under this condition, the chlorogenic acid content reached 0.35%. The extraction conditions of the ultrasonic extraction method were as follows: pre-impregnation of 60% ethanol with a liquid-solid ratio of 15:1 for 40 min, and ultrasonic extraction for 45 min. Under this condition, the mass fraction of chlorogenic acid reached 0.36%.
In the water bath method and the ultrasonic method, the main factors affecting the extraction of chlorogenic acid are basically the same, and the difference is that the extraction effect under ultrasonic conditions is better than that of the water bath. The reasons may be as follows: 1 the destruction of the cell membrane by the cavitation of the ultrasonic wave contributes to the release and dissolution of the chlorogenic acid; 2 the ultrasonic wave causes the extracting agent and the extract to continuously oscillate, contributing to the diffusion of the solute; 3 the thermal effect of the ultrasound makes The temperature of the aqueous medium was maintained at 60 ° C, and the sample had a water bath effect.
Application: used in AKD Emulsifier
Product Type: Cassava starch imported from China
Chemical composition: Tapioca starch
Appearance:White powder
Moisture ( % ): ≤ 14.0
Spots ( a / cm2): ≤ 2
Viscosity: 20 ~ 50 s (20%, 40 °C, 4 # Tu's cup)
pH value: 6.0 ~ 7.5
Toxicity: No harm to human health during operation and use
Storage: Store in a cool , dry, ventilated warehouse
Nature: white, gelatinization in low temperature , good fluidity , viscosity stability, aging resistance , the film is good , strong bond , fast drying . Products with low protein content , gelatinization liquid not perishable , no foam , no smell. Good adhesion properties of various fibers , high compatibility with other additives . For AKD emulsifier, the rational use of the product can effectively ensure emulsifying effect and reduce production cost.
Dosage: Production of one ton of 25% emulsifier simply add 192kg of the product
Packing: 25 kg / bag.
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AKD Special Starch
Akd Special Starch,Oxidized Starch,Starch For Akd Emulsifer,Cassava Starch
Shandong Tiancheng Chemical Co., Ltd. , https://www.tianchengchemical.com