CN105784539A - Trihydroxyl diphenylethanone test method - Google Patents

Trihydroxyl diphenylethanone test method Download PDF

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Publication number
CN105784539A
CN105784539A CN201610339138.3A CN201610339138A CN105784539A CN 105784539 A CN105784539 A CN 105784539A CN 201610339138 A CN201610339138 A CN 201610339138A CN 105784539 A CN105784539 A CN 105784539A
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CN
China
Prior art keywords
content detection
inspection
phenyl ketone
benzyl phenyl
trihydroxy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610339138.3A
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Chinese (zh)
Inventor
沈少银
袁玲
肖兴亮
王军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhu Baoping Intelligent Service Outsourcing Co Ltd
Original Assignee
Wuhu Baoping Intelligent Service Outsourcing Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhu Baoping Intelligent Service Outsourcing Co Ltd filed Critical Wuhu Baoping Intelligent Service Outsourcing Co Ltd
Priority to CN201610339138.3A priority Critical patent/CN105784539A/en
Publication of CN105784539A publication Critical patent/CN105784539A/en
Pending legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
    • G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a trihydroxyl diphenylethanone test method which comprises content detection and moisture detection, wherein the content detection comprises an impurity removal step and a detection step, and the impurity removal step comprises the following steps: accurately weighing 1-10g of sample in a conical flask (containing 50mu g of trihydroxyl diphenylethanone; adding 40ml of absolute ethyl alcohol and adding 2ml of glacial acetic acid (0.05M) while shaking; filtering; and fetching the filtrate and introducing the sample. Compared with the prior art, the method disclosed by the invention has the advantages that the content detection and moisture detection of trihydroxyl diphenylethanone are added, and the repeatability RSD of the content detection is 4-8%.

Description

A kind of method of inspection of trihydroxy benzyl phenyl ketone
Technical field
The invention belongs to the method for inspection of chemical intermediate, particularly belong to trihydroxy benzyl phenyl ketone The method of inspection.
Background technology
Daidzein semi-finished product trihydroxy benzyl phenyl ketone Content, moisture the quality of daidzein is had a serious impact, the most still there is no inspection party Its quality is tested by method.
Summary of the invention
The technical problem to be solved is to provide a kind of new trihydroxy benzyl phenyl ketone The method of inspection.
The present invention solves the technical scheme of technical problem: the inspection of a kind of trihydroxy benzyl phenyl ketone Method, including content detection, water content detection, described content detection comprises the following steps: remove Miscellaneous step, detecting step, described removal step is for accurately to weigh 1-10 gram of sample in triangle (containing trihydroxy benzyl phenyl ketone 50ug in Ping；), add 40ml dehydrated alcohol, add 2ml ice vinegar The edged shaking of acid (0.05M) limit；Filter, take subsequent filtrate sample introduction；
Described detecting step is, uses the external standard method in high performance liquid chromatography, chromatographic condition Being 254 for detection wavelength, flowing is absolute methanol solution mutually.
Described water content detection is: weighs 1g sample (accurate to 0.0002g) and is placed in constant weight in advance Weighing botle in, put in the drying baker of modulated to 105 DEG C ± 2 DEG C and dry to constant weight, move into dry It is cooled to room temperature in dry device, weighs.
The present invention compared with prior art, adds content detection and the water of trihydroxy benzyl phenyl ketone Go-on-go is surveyed, and the repeated RSD of content detection is 4-8%.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1:
The method of inspection of a kind of trihydroxy benzyl phenyl ketone, including content detection, water content detection, institute The content detection stated comprises the following steps: removal step, detecting step, described removal step For accurately weighing 1-10 gram of sample in triangular flask (containing trihydroxy benzyl phenyl ketone 50ug；), add 40ml dehydrated alcohol, adds the edged shaking of 2ml glacial acetic acid (0.05M) limit；Filter, take continuous Filtrate sample introduction；
Described detecting step is, uses the external standard method in high performance liquid chromatography, chromatographic condition Being 254 for detection wavelength, flowing is absolute methanol solution mutually.
Repeating above-mentioned test 6 times, its repeatability RSD is 6%.Described water content detection is: Weigh 1g sample (accurate to 0.0002g) to be placed in the weighing botle of constant weight in advance, put into modulated Dry to constant weight to the drying baker of 105 DEG C ± 2 DEG C, in moving into exsiccator, be cooled to room temperature, claim Weight.
Moisture content percentage composition (X) is calculated as follows:
X = m 1 - m 2 m 1 × 100
In formula: m1Sample mass g before drying；
m2Sample mass g after baking；
X water content.
The fusing point of described trihydroxy benzyl phenyl ketone is 180-188 DEG C, molten away from≤4 DEG C, moisture content ≤ 0.5%.

Claims (4)

1. a method of inspection for trihydroxy benzyl phenyl ketone, including content detection, water content detection.
The method of inspection of a kind of trihydroxy benzyl phenyl ketone the most according to claim 1, its It is characterised by: described content detection comprises the following steps: removal step, detecting step, institute The removal step stated is for accurately to weigh 1-10 gram of sample in triangular flask (containing trihydroxy hexichol second Ketone 50ug；), add 40ml dehydrated alcohol, add the edged shaking of 2ml glacial acetic acid (0.05M) limit； Filter, take subsequent filtrate sample introduction.
The method of inspection of a kind of trihydroxy benzyl phenyl ketone the most according to claim 2, its It is characterised by:
Described detecting step is, uses the external standard method in high performance liquid chromatography, chromatographic condition Being 254 for detection wavelength, flowing is absolute methanol solution mutually.
The method of inspection of a kind of trihydroxy benzyl phenyl ketone the most according to claim 1, its It is characterised by: described water content detection is: weigh 1g sample (accurate to 0.0002g) and be placed in pre- In the weighing botle of first constant weight, put in the drying baker of modulated to 105 DEG C ± 2 DEG C and dry to constant weight, It is cooled to room temperature in moving into exsiccator, weighs.
CN201610339138.3A 2016-05-20 2016-05-20 Trihydroxyl diphenylethanone test method Pending CN105784539A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610339138.3A CN105784539A (en) 2016-05-20 2016-05-20 Trihydroxyl diphenylethanone test method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610339138.3A CN105784539A (en) 2016-05-20 2016-05-20 Trihydroxyl diphenylethanone test method

Publications (1)

Publication Number Publication Date
CN105784539A true CN105784539A (en) 2016-07-20

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610339138.3A Pending CN105784539A (en) 2016-05-20 2016-05-20 Trihydroxyl diphenylethanone test method

Country Status (1)

Country Link
CN (1) CN105784539A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6166142A (en) * 1984-09-07 1986-04-04 Kaneko Agricult Mach Co Ltd Moisture measuring method of livestock manure
CN101210907A (en) * 2006-12-28 2008-07-02 天津市食品研究所有限公司 Wheat flour benzoyl peroxide highly effective liquid phase chromatography detection method
CN103439288A (en) * 2013-08-24 2013-12-11 浙江大学 Real-time release detection method for ginkgo leaf medicinal material
CN104237060A (en) * 2014-10-05 2014-12-24 浙江大学 Multi-index quick detection method of honeysuckle
CN104374862A (en) * 2014-11-27 2015-02-25 成都大学 Salvia miltiorrhiza stem leaf quality control method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6166142A (en) * 1984-09-07 1986-04-04 Kaneko Agricult Mach Co Ltd Moisture measuring method of livestock manure
CN101210907A (en) * 2006-12-28 2008-07-02 天津市食品研究所有限公司 Wheat flour benzoyl peroxide highly effective liquid phase chromatography detection method
CN103439288A (en) * 2013-08-24 2013-12-11 浙江大学 Real-time release detection method for ginkgo leaf medicinal material
CN104237060A (en) * 2014-10-05 2014-12-24 浙江大学 Multi-index quick detection method of honeysuckle
CN104374862A (en) * 2014-11-27 2015-02-25 成都大学 Salvia miltiorrhiza stem leaf quality control method

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Application publication date: 20160720