Brazilian green propolis quality control method

A quality control method, the technology of propolis, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that it is difficult to ensure the effectiveness and stability of propolis, no correlation of curative effect, different fingerprints, etc.

CN105929074AActive Publication Date: 2016-09-07ZHEJIANG UNIV +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2016-09-07

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Abstract

The invention provides a Brazilian green propolis quality control method. The Brazilian green propolis quality control method is implemented through the following steps that a test propolis sample is ultrasonically extracted with ethyl alcohol, filtered and detected through high performance liquid chromatography, the content of six evaluation index ingredients is calculated according to a standard curve, and whether the quality of Brazilian green propolis is high or low is evaluated through the content of the six ingredients, that is to say, if the total sum of the content of the six ingredients is larger than 10%, the Brazilian green propolis is high-quality propolis, and if the total sum of the content of the six ingredients is smaller than 6%, the Brazilian green propolis is low-quality propolis. According to the method, the chemical ingredients of the Brazilian green propolis are combined with the antioxidant activity, the antioxidant material basis of the Brazilian green propolis is illustrated, the defect that some main ingredients do not achieve the high pharmacological activity is avoided, and the antioxidant activity of the Brazilian green propolis can be reflected more truly; the design is reasonable, the irrationality that in an existing method, total flavonoid is taken as the quality control index of the Brazilian green propolis is overcome, the defect that content detection of multiple flavones or phenolic acids has no correlation with the activity is overcome, and a novel method is provided for Brazilian green propolis quality control.
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Description

technical field

[0001] The invention belongs to the field of propolis quality control and relates to a method for controlling the quality of Brazilian green propolis. Background technique

[0002] Brazilian green propolis is collected from the southeastern and central western regions of Brazil, and its plant source is Baccharis dracunculifolia DC. It is one of the most popular and researched types of propolis at home and abroad, and has been widely used in health food to improve human Health and disease prevention.

[0003] Brazilian green propolis has been imported to China for more than ten years. Due to the lack of quality evaluation methods, we can only refer to the national standard of Chinese propolis and use the total flavonoid content as the quality control index. The main components of Brazilian green propolis are prenylated phenylpropanoids and prenyl derivatives of p-coumaric acid, and the content of flavonoids is relatively low. Obviously, taking the total flav...

Examples

Embodiment 1

[0017] (1) Propolis sample preparation

[0018] Take 3 samples of Brazilian green propolis from different batches, freeze and pulverize them, and use 95% ethanol for ultrasonic extraction for 30 minutes. Dilute to 50mL, filter through a microporous membrane to obtain S1, S2, and S3 detection sample solutions respectively.

[0019] (2) HPLC detection

[0020] Conditions: Sepax HP-C18 (150mm*4.6mm, 5μm); mobile phase: methanol-0.1% acetic acid; flow rate: 1.0mL / min; wavelength: 280nm. Column temperature: 33°C. Injection volume: 5 μL. The optimized gradient elution program is: 0-10min, 15-25% methanol; 10-25min, 25-40% methanol; 25-55min, 40-60% methanol; 55-75min, 60-75% methanol; 75 -90min, 75-85% methanol.

[0021] (3) Offline HPLC-DPPH analysis

[0022] Pipette S1, S2, and S3 propolis alcohol extracts respectively, add freshly prepared DPPH ethanol solution, react in the dark for a period of time at room temperature, and filter through a filter membrane as the experimen...

Embodiment 2

[0032] (1) Propolis sample preparation

[0033] Take 3 samples of Brazilian green propolis from different batches, freeze and pulverize them, and use 70% ethanol for ultrasonic extraction for 45 minutes. The ratio of solid to liquid is 1:30. Dilute to 50mL, filter through a microporous membrane to obtain S4, S5, and S6 detection sample solutions respectively.

[0034] (2) High performance liquid chromatography detection conditions

[0035] Sepax HP-C18 (150mm*4.6mm, 5μm); mobile phase: methanol-0.1% acetic acid; flow rate: 1.0mL / min; wavelength: 280nm. Column temperature: 33°C. Injection volume: 5 μL. The optimized gradient elution program is: 0-10min, 15-25% methanol; 10-25min, 25-40% methanol; 25-55min, 40-60% methanol; 55-75min, 60-75% methanol; 75 -90min, 75-85% methanol.

[0036] (3) Quality evaluation of antioxidant activity of Brazilian green propolis

[0037] Calculation of chlorogenic acid, caffeic acid, 3,5-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, 3,4,...

Embodiment 3

[0041] (1) Propolis sample preparation

[0042] Take 3 samples of Brazilian green propolis from different batches, freeze and pulverize them, and use 85% ethanol for ultrasonic extraction for 45 minutes. The ratio of solid to liquid is 1:10. Dilute to 50mL, filter through microporous membrane to obtain S7, S8, S9 testing sample solutions respectively.

[0043] (2) High performance liquid chromatography detection conditions

[0044] Sepax HP-C18 (150mm*4.6mm, 5μm); mobile phase: methanol-0.1% acetic acid; flow rate: 1.0mL / min; wavelength: 280nm. Column temperature: 33°C. Injection volume: 5 μL. The optimized gradient elution program is: 0-10min, 15-25% methanol; 10-25min, 25-40% methanol; 25-55min, 40-60% methanol; 55-75min, 60-75% methanol; 75 -90min, 75-85% methanol.

[0045](3) Quality evaluation of antioxidant activity of Brazilian green propolis

[0046] Calculation of chlorogenic acid, caffeic acid, 3,5-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, 3,4,5-tricaff...