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A kind of separation and purification method of unstable crocin
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A technology for separation and purification of crocin, which is applied in the field of medicine and can solve the problems that the quality of crocus medicinal materials cannot be fully reflected.
Active Publication Date: 2021-06-18
上海诗丹德标准技术服务有限公司
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Problems solved by technology
The 2015 edition of "Chinese Pharmacopoeia" only recorded crocin-I and glycoside-II in crocin as indicators for quality control of saffron, but only crocin-I and crocin The total content of glucoside-II is the standard and cannot fully reflect the quality of saffron
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Embodiment 1
[0101] Example 1 Separation and purification of unstable crocin monomer compound Crocin III
[0102] After the dried saffron sample (55g) is pulverized, add 30 times of dilute ethanol solution according to mass / volume, avoid light and ultrasonic (1.5h / time), extract once, avoid light and filter, combine the filtrate, and keep away from light at 45°C. Concentrate lightly to no alcohol, and freeze-dry to obtain a freeze-dried crude extract sample.
[0103] The crude extract sample was dissolved in 50% methanol water, centrifuged at 12000rpm for 5min to obtain a supernatant; the supernatant was subjected to medium pressure column chromatography (Pump200, 100*460mm, C 18 Filler 40-60μm), detection wavelength 254nm, 330nm and 440nm, flow rate 70mL / min. First use 30% methanol water to elute, collect the eluate according to the peak and record it as component Fr.1; then change to 50% methanol water for elution, collect the eluate according to the peak, and record it as component Fr....
Embodiment 2
[0108] Example 2 Separation and purification of unstable crocin monomer compound crocetin monoglucose ester
[0109] After the dried saffron sample (55g) is pulverized, add 30 times of dilute ethanol solution according to mass / volume, avoid light and ultrasonic (1.5h / time), extract once, avoid light and filter, combine the filtrate, and keep away from light at 45°C. Concentrate lightly to no alcohol, and freeze-dry to obtain a freeze-dried crude extract sample.
[0110]The crude extract sample was dissolved in 50% methanol water, centrifuged at 12000rpm for 5min to obtain a supernatant; the supernatant was subjected to medium pressure column chromatography (Pump200, 100*460mm, C 18 Filler 40-60μm), detection wavelength 254nm, 330nm and 440nm, flow rate 70mL / min. First use 30% methanol water to elute, collect the eluent according to the peak and record it as component Fr.1; then replace it with 50% methanol water for isocratic elution, collect the eluent according to the peak,...
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Abstract
The invention relates to a method for separating and purifying unstable crocin, belonging to the technical field of medicine. Specifically, the present invention provides a method for separation and purification of crocin monomers, including extraction, concentration, freeze-drying, separation and purification. The whole technological process is easy to operate, the operating conditions are easy to control, and the operation steps are easy to repeat, and high-purity crocin monomer compounds crocin-III and crocetin monoglucose ester with poor stability can be separated and prepared.
Description
technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for separating and purifying unstable crocin. Background technique [0002] The medicinal material of saffron is the dry stigma of Crocus sativus L., also known as saffron and saffron. Its use value is clear, and at the same time, it is also an important raw material in the field of consumer goods such as high-end cosmetics, spices and dyes. Due to its special use, extremely low output, and high price, it is a rare and precious medicinal material, known as "plant gold". Saffron is native to the Mediterranean coast, Central Asia and West Asia, and was introduced into my country via Tibet. At present, it has been introduced and cultivated in various provinces and cities in southern my country. Shanghai, Zhejiang, Jiangsu, etc., as one of the important domestic producing areas of saffron, have been planting since the 1960s and 1970s, but most of the planting i...
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