CN105954408A - Detection method for detecting plasticizers in traditional Chinese medicine grease - Google Patents
Detection method for detecting plasticizers in traditional Chinese medicine grease Download PDFInfo
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- CN105954408A CN105954408A CN201610272115.5A CN201610272115A CN105954408A CN 105954408 A CN105954408 A CN 105954408A CN 201610272115 A CN201610272115 A CN 201610272115A CN 105954408 A CN105954408 A CN 105954408A
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- chinese medicine
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- 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
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- 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
- G01N2030/025—Gas chromatography
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Abstract
The invention discloses a detection method for detecting plasticizers in the traditional Chinese medicine grease. The method comprises the steps of metering the volume, purifying, metering the volume again and conducting the gas chromatography-mass spectrometry detection. Compared with the prior art, the method of the present invention has the following advantages: (1) based on the detection method for detecting plasticizers in the traditional Chinese medicine grease, plasticizers, which are wider in the range of molecular weights and polarities, can be identified and quantified at a high sensitivity through the single analysis; (2) the detection method is wider in the range of compound types that can be detected.
Description
Technical field
The invention belongs to analytical chemistry field, relate to the detection of plasticiser, particularly relate to the detection of plasticiser in a kind of Chinese medicine oils and fats
Method.
Background technology
Plasticiser, the most also referred to as plasticizer.Plasticizer is the industrial macromolecular material auxiliary agent being widely used, in plastic processing
This material of middle interpolation, can make its pliability strengthen, be easily worked, can be legal for industrial use.TaiWan, China manufacturer uses
A kind of common plasticizer DEHP (then detect DINP, DNOP, DBP, DMP, DEP etc. successively) replaces Petiolus Trachycarpi oil to join
The mist generating agent of system also can produce the thickening effect similar with emulsifying agent.But, insider points out, DEHP, DINP etc. plastify
Agent is also not belonging to food flavor raw material.Therefore, DEHP not only cannot function as a kind of kasher additive, even can not use
In packaging for foodstuff." mist generating agent " is a kind of legal food additive, is frequently used in the food such as fruit juice, fruit jam, beverage,
It is made up of arabic gum, emulsifying agent, Petiolus Trachycarpi oil and numerous food additives mixed.
Phthalate (Phthalic acid esters, PAEs) is the plasticiser that industry is conventional, is used for increasing plastic
Plasticity and toughness, improve plastic intensity.Its molecule is with phthalic acid as parent nucleus, and lipotropy is strong, in the plastic
Not combining with covalent bond, therefore when alcohol exposure, oils composition, plasticiser will dissolve in.Plasticiser in plastics
Content is the highest, and the plasticiser quantity that can be dissolved is the biggest.Phthalic acid ester is a class environmental hormone, and its acute toxicity does not show
Write, but liver, kidney, lung and heart, reproductive system are all had infringement.There are research display, the absorption of phthalate
The normal of children's intelligence and behavior can be affected.The Chinese medicine oils and fats sold currently on the market is all based on plastic bottle/barreled, adjacent benzene
The migration during storing of the diformic ester plasticiser is a potential safety hazard of Chinese medicine oils and fats, is also asking of easily ignoring of people
Topic.Owing to oils substrate is special, when using instrument detection, ambient interferences is relatively big, detects relatively difficult.
The method of plasticiser in oils and fats that detects in prior art has multiple, but Chinese medicine oils and fats is owing to wherein containing different Chinese drug-treated group
Point, therefore detect more difficulty.
Summary of the invention
Present invention solves the technical problem that and be: in order to overcome the defect of prior art, it is thus achieved that one can rapid sensitive detection oils and fats
The method of middle plasticiser, the invention provides the detection method of plasticiser in a kind of Chinese medicine oils and fats.
Technical scheme: the detection method of plasticiser in a kind of Chinese medicine oils and fats, comprises the steps of
(1) measure Chinese medicine oils and fats 1～12 μ L, be settled to 5～10mL by ethyl acetate, vortex oscillation 1～5 minutes；Take 1～
The mixed liquor hexamethylene of 3mL is settled to 3～6mL, vortex oscillation 2～6 minutes；
(2) the product oil bath that step (1) obtains being evaporated, again with methanol is settled to 1～3mL, uses gel permeation chromatography
Purify, wherein sample size be 1～1.5mL, flow velocity be 2～4mL/min, effluent acquisition time be 25～60 minutes；
(3) 3～6mL will be settled in the product after step (2) purification adds Ethyl acetate-cyclohexane mixed liquor,
Wherein ethyl acetate is 1.5～3:1 with the volume ratio of hexamethylene；
(4) product using gas chromatography-mass spectrum to obtain step (3) detects, and wherein GC conditions is: carrier gas
For nitrogen, flow velocity be 1～1.5mL/min, inlet temperature be 245～255 DEG C；Mass Spectrometry Conditions is: interface temperature 280～290 DEG C,
Ionizing energy 68～75eV.
Preferably, step (1) measures Chinese medicine oils and fats 8 μ L, be settled to 7mL, vortex oscillation 4 minutes by ethyl acetate；Take
The mixed liquor hexamethylene of 2mL is settled to 5mL, vortex oscillation 5 minutes.
Preferably, the product oil bath that step (1) obtains being evaporated in step (2), again with methanol is settled to 2mL, uses solidifying
Glue penetration chromatographic purification, wherein sample size be 1.3mL, flow velocity be 3mL/min, effluent acquisition time be 40 minutes.
Preferably, step (3) will add in Ethyl acetate-cyclohexane mixed liquor through the product after step (2) purification,
Being settled to 5mL, wherein ethyl acetate is 2.5:1 with the volume ratio of hexamethylene.
Preferably, the product using gas chromatography-mass spectrum to obtain step (3) in step (4) detects, wherein gas phase color
Spectral condition is: carrier gas be nitrogen, flow velocity be 1.2mL/min, inlet temperature be 250 DEG C；Mass Spectrometry Conditions is: interface temperature 286 DEG C,
Ionizing energy 72eV.
Beneficial effect: (1) present invention provide Chinese medicine oils and fats in plasticiser detection method can single analyze in high sensitivity
Ground is identified and quantitative wider molecular weight ranges and the plasticiser of polarity scope；(2) plasticiser in the Chinese medicine oils and fats that the present invention provides
The classes of compounds of detection method detection is wider.
Detailed description of the invention
Embodiment 1
In a kind of Chinese medicine oils and fats, the detection method of plasticiser, comprises the steps of
(1) measure Chinese medicine oils and fats 1 μ L, be settled to 5mL, vortex oscillation 1 minute by ethyl acetate；Take the mixed liquor of 1mL
It is settled to 3mL, vortex oscillation 2 minutes with hexamethylene；
(2) the product oil bath that step (1) obtains being evaporated, again with methanol is settled to 1mL, uses gel permeation chromatography to purify,
Wherein sample size be 1mL, flow velocity be 2mL/min, effluent acquisition time be 25 minutes；
(3) 3mL will be settled in the product after step (2) purification adds Ethyl acetate-cyclohexane mixed liquor, its
Middle ethyl acetate is 1.5:1 with the volume ratio of hexamethylene；
(4) product using gas chromatography-mass spectrum to obtain step (3) detects, and wherein GC conditions is: carrier gas
For nitrogen, flow velocity be 1mL/min, inlet temperature be 245 DEG C；Mass Spectrometry Conditions is: interface temperature 280 DEG C, ionizing energy 68eV.
Embodiment 2
In a kind of Chinese medicine oils and fats, the detection method of plasticiser, comprises the steps of
(1) measure Chinese medicine oils and fats 8 μ L, be settled to 7mL, vortex oscillation 4 minutes by ethyl acetate；Take the mixed liquor of 2mL
It is settled to 5mL, vortex oscillation 5 minutes with hexamethylene；
(2) the product oil bath that step (1) obtains being evaporated, again with methanol is settled to 2mL, uses gel permeation chromatography to purify,
Wherein sample size be 1.3mL, flow velocity be 3mL/min, effluent acquisition time be 40 minutes；
(3) 5mL will be settled in the product after step (2) purification adds Ethyl acetate-cyclohexane mixed liquor, its
Middle ethyl acetate is 2.5:1 with the volume ratio of hexamethylene；
(4) product using gas chromatography-mass spectrum to obtain step (3) detects, and wherein GC conditions is: carrier gas
For nitrogen, flow velocity be 1.2mL/min, inlet temperature be 250 DEG C；Mass Spectrometry Conditions is: interface temperature 286 DEG C, ionizing energy
72eV。
Embodiment 3
In a kind of Chinese medicine oils and fats, the detection method of plasticiser, comprises the steps of
(1) measure Chinese medicine oils and fats 12 μ L, be settled to 10mL, vortex oscillation 5 minutes by ethyl acetate；Take the mixing of 3mL
Liquid hexamethylene is settled to 6mL, vortex oscillation 6 minutes；
(2) the product oil bath that step (1) obtains being evaporated, again with methanol is settled to 3mL, uses gel permeation chromatography to purify,
Wherein sample size be 1.5mL, flow velocity be 4mL/min, effluent acquisition time be 60 minutes；
(3) 6mL will be settled in the product after step (2) purification adds Ethyl acetate-cyclohexane mixed liquor,
Wherein ethyl acetate is 3:1 with the volume ratio of hexamethylene；
(4) product using gas chromatography-mass spectrum to obtain step (3) detects, and wherein GC conditions is: carrier gas
For nitrogen, flow velocity be 1.5mL/min, inlet temperature be 255 DEG C；Mass Spectrometry Conditions is: interface temperature 290 DEG C, ionizing energy
75eV。
Using the detection method described in embodiment 1～3 to detect the plasticiser in Chinese medicine oils and fats, result is as shown in the table:
Claims (5)
1. the detection method of plasticiser in a Chinese medicine oils and fats, it is characterised in that comprise the steps of
(1) measure Chinese medicine oils and fats 1～12 μ L, be settled to 5～10mL by ethyl acetate, vortex oscillation 1～5 minutes；Take 1～
The mixed liquor hexamethylene of 3mL is settled to 3～6mL, vortex oscillation 2～6 minutes；
(2) the product oil bath that step (1) obtains being evaporated, again with methanol is settled to 1～3mL, uses gel permeation chromatography
Purify, wherein sample size be 1～1.5mL, flow velocity be 2～4mL/min, effluent acquisition time be 25～60 minutes；
(3) 3～6mL will be settled in the product after step (2) purification adds Ethyl acetate-cyclohexane mixed liquor,
Wherein ethyl acetate is 1.5～3:1 with the volume ratio of hexamethylene；
(4) product using gas chromatography-mass spectrum to obtain step (3) detects, and wherein GC conditions is: carrier gas
For nitrogen, flow velocity be 1～1.5mL/min, inlet temperature be 245～255 DEG C；Mass Spectrometry Conditions is: interface temperature 280～290 DEG C,
Ionizing energy 68～75eV.
The detection method of plasticiser in a kind of Chinese medicine oils and fats the most according to claim 1, it is characterised in that amount in step (1)
Take Chinese medicine oils and fats 8 μ L, be settled to 7mL, vortex oscillation 4 minutes by ethyl acetate；Take the mixed liquor hexamethylene of 2mL
It is settled to 5mL, vortex oscillation 5 minutes.
The detection method of plasticiser in a kind of Chinese medicine oils and fats the most according to claim 1, it is characterised in that will in step (2)
The product oil bath that step (1) obtains is evaporated, and again with methanol is settled to 2mL, uses gel permeation chromatography to purify, Qi Zhongjin
Sample amount is 1.3mL, flow velocity is 3mL/min, effluent acquisition time is 40 minutes.
The detection method of plasticiser in a kind of Chinese medicine oils and fats the most according to claim 1, it is characterised in that will in step (3)
Product after step (2) purification adds in Ethyl acetate-cyclohexane mixed liquor, is settled to 5mL, wherein acetic acid second
Ester is 2.5:1 with the volume ratio of hexamethylene.
The detection method of plasticiser in a kind of Chinese medicine oils and fats the most according to claim 1, it is characterised in that step is adopted in (4)
The product obtained step (3) with gas chromatography-mass spectrum detects, and wherein GC conditions is: carrier gas be nitrogen,
Flow velocity is 1.2mL/min, inlet temperature is 250 DEG C；Mass Spectrometry Conditions is: interface temperature 286 DEG C, ionizing energy 72eV.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610272115.5A CN105954408A (en) | 2016-04-28 | 2016-04-28 | Detection method for detecting plasticizers in traditional Chinese medicine grease |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610272115.5A CN105954408A (en) | 2016-04-28 | 2016-04-28 | Detection method for detecting plasticizers in traditional Chinese medicine grease |
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| CN105954408A true CN105954408A (en) | 2016-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610272115.5A Pending CN105954408A (en) | 2016-04-28 | 2016-04-28 | Detection method for detecting plasticizers in traditional Chinese medicine grease |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112305110A (en) * | 2020-10-26 | 2021-02-02 | 舟山新诺佳生物工程有限责任公司 | Detection method suitable for ethyl ester type and glyceride type fish oil product plasticizers |
-
2016
- 2016-04-28 CN CN201610272115.5A patent/CN105954408A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 熊瑛等: "中药油脂中邻苯二甲酸酯类塑化剂的检测分析", 《中国油脂》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112305110A (en) * | 2020-10-26 | 2021-02-02 | 舟山新诺佳生物工程有限责任公司 | Detection method suitable for ethyl ester type and glyceride type fish oil product plasticizers |
| CN112305110B (en) * | 2020-10-26 | 2022-08-12 | 舟山新诺佳生物工程有限责任公司 | Detection method suitable for ethyl ester type and glyceride type fish oil product plasticizers |
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Application publication date: 20160921 |
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