CN104764817A - Method for detecting atranol compound in cosmetic - Google Patents
Method for detecting atranol compound in cosmetic Download PDFInfo
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Abstract
The invention discloses a method for detecting an atranol compound in a cosmetic. The method comprises the following steps: adding an aqueous solution of ammonium acetate into a sample to be detected, adding a 5% trichloroacetic acid-acetonitrile solution, carrying out ultrasonic extraction, centrifuging the above obtained extract liquid, taking the obtained supernatant, allowing the supernatant to go through a millipore filtration membrane, and carrying out high performance liquid chromatography determination. An ultraviolet detector is adopted to detect, and the detection wavelength is 280nm. The method for determining the atranol compound and chloroatranol in the cosmetic through high performance liquid chromatography has the advantages of rapidness, simple pretreatment, low detection limit and high recovery rate.
Description
Technical field
The invention belongs to analysis of cosmetics field, be specifically related to a kind of method detecting γ-orcylaldehyde compound in cosmetics.
Background technology
Lichens (lichens) colonizes in the symbiosis complex organisms that a kind of fungi (fungi) on trunk and algae (algae) highly combine, containing a large amount of depsides, depsidone and lipoid substance, through effects such as hydrolysis, alcoholysis or decarboxylations, can produce the Small molecular list aryl compound with peculiar fragrance, be a kind of very important natural perfume material.On international natural perfume material market, lichens spices can be divided into oak moss (oak moss) extract and tree moss (tree moss) extract two class, is requisite aroma source in the well-known classical perfume recipe of many moneys.
EU Committee proposes 26 kinds of sensibiligens (comprising 24 kinds of compounds and 2 kinds of natural extracts) the highest limitation in cosmetics in regulatory affairs (Council Directive 76/768/EEC) the 7th amendment, require that its content must not higher than 0. 001% in resident class cosmetics, in non-resident class cosmetics, content must not higher than 0. 01%.γ-orcylaldehyde (chemical name 2,6-dihydroxy-4-tolyl aldehyde, CAS 526-37-4) and chlorination γ-orcylaldehyde (chemical name 3-chloro-2,6-dihydroxy-4-tolyl aldehyde, CAS 57074-21-2) two kinds of γ-orcylaldehyde compounds are two kinds of core flavor components in 2 kinds of natural extracts (tree moss natural extract and oak moss natural extract) of using of restriction, existing many sections of bibliographical informations its there is sensitization.According to the data of consumer safety Science committee of European Union, existing many sensitization cases occur, and about have the crowd of 1% ~ 3% can produce allergic symptom to this constituents, cause chafing, eruption or dry and cracked.In July, 2014, European Union announced, due to may allergy be caused, and formal forbidding γ-orcylaldehyde compound from 2015.
In order to protect cosmetics consumption safety, the use of sensitization aromatic γ-orcylaldehyde or chlorination γ-orcylaldehyde in effective monitoring cosmetics, the composition adopting effective means to detect γ-orcylaldehyde or chlorination γ-orcylaldehyde in cosmetics is crucial.The many employings of prior art utilize gas chromatography-mass spectrum (GC-MS) to analyze γ-orcylaldehyde or chlorination γ-orcylaldehyde in cosmetics, but need first to derive, complex operation, be difficult to meet the needs of express-analysis in real work.
Summary of the invention
The object of this invention is to provide a kind of method detecting γ-orcylaldehyde compound in cosmetics, the method sample pre-treatments is simple and efficient, detectability is low, and the recovery is high; Effectively can detect the γ-orcylaldehyde in cosmetics or chlorination γ-orcylaldehyde, for cosmetic product quality control and product safety monitor the support that provides the necessary technical, thus the consumption safety of protection cosmetics.
For achieving the above object, the technical solution used in the present invention is: a kind of method detecting γ-orcylaldehyde compound in cosmetics, comprises the steps:
(1) sample to be tested is added in ammonium acetate aqueous solution, add the mixed extract that trichloroacetic acid solution and acetonitrile form after vortex again, then through vortex, ultrasonic extraction, obtain extract;
(2) extract is centrifugal, get supernatant micro-pore-film filtration and obtain extract solution;
(3) using acetonitrile and water as mobile phase, high efficiency liquid phase chromatographic analysis method is utilized to detect described extract solution; UV-detector is adopted to detect when carrying out efficient liquid phase chromatographic analysis.
In technique scheme, in step (1), the concentration of ammonium acetate aqueous solution is 0.02 mol/L; The consumption of corresponding every gram of sample to be tested ammonium acetate aqueous solution is 0.75mL.
In technique scheme, in step (1), the time of vortex first time is 30 s; The time of second time vortex is 60 s; Ultrasonic extraction time is 15 min.
In technique scheme, in step (1), in trichloroacetic acid solution, the massfraction of trichloroacetic acid is 5%; In the mixed extract that trichloroacetic acid solution and acetonitrile form, the volume ratio of trichloroacetic acid solution, acetonitrile is 75: 25.
In technique scheme, in step (2), rotating speed time centrifugal is 10000 rpm, and the time is 10 min; The aperture of microporous barrier is 0.22 μm.
In technique scheme, when adopting UV-detector to detect, determined wavelength is 280 nm.
In technique scheme, adopt gradient elution during efficient liquid phase chromatographic analysis extract solution in step (3), Gradient program is: 0 ~ 8 min, 25 ~ 90 % acetonitriles; 8 ~ 11 min, 90 % acetonitriles; 11 ~ 14 min, 25 % acetonitriles.
In the present invention, γ-orcylaldehyde compound is γ-orcylaldehyde or chlorination γ-orcylaldehyde, can detect in cosmetics whether contain γ-orcylaldehyde compound, also can obtain the content of γ-orcylaldehyde compound in cosmetics according to high performance liquid chromatography.For γ-orcylaldehyde, concrete grammar is, adopts γ-orcylaldehyde standard items to obtain the peak area at the corresponding peak of γ-orcylaldehyde that high performance liquid chromatography under different γ-orcylaldehyde concentration detects by efficient liquid phase chromatographic analysis, preparation standard curve; Then high performance liquid chromatography detection is carried out to the extract solution of sample to be tested, obtain the peak area at its corresponding peak, then contrast with typical curve the concentration obtaining γ-orcylaldehyde in sample to be tested, then through calculating the content of γ-orcylaldehyde in cosmetics; Wherein, the acetonitrile-aqueous solution that γ-orcylaldehyde can be diluted to variable concentrations gradient by γ-orcylaldehyde standard items is made.γ-orcylaldehyde is changed to chlorination γ-orcylaldehyde, also can draws the content of chlorination γ-orcylaldehyde in cosmetics.
The mass concentration treating γ-orcylaldehyde or chlorination γ-orcylaldehyde in sample measuring liquid is obtained, then according to γ-orcylaldehyde in following formulae discovery cosmetics or chlorination γ-orcylaldehyde content by high efficiency liquid phase chromatographic analysis method:
In formula:
W---γ-orcylaldehyde or chlorination γ-orcylaldehyde massfraction in cosmetics, mg/kg;
c---the mass concentration of γ-orcylaldehyde or chlorination γ-orcylaldehyde in testing sample, mg/L;
v---sample constant volume, mL;
m---amount of samples, g.
Adopt technique scheme, be limited to 5 mg/kg to detecting of γ-orcylaldehyde compound in cosmetics, the recovery is 77.4 ~ 96.3 %, and relative standard deviation (RSD) is 1.41 ~ 4.63 %.
In the present invention, γ-orcylaldehyde, chlorination γ-orcylaldehyde chemical structural formula are similar, the condition detected for liquid chromatography, ultraviolet light is also close, carries out one-time detection and can learn in cosmetics whether contain γ-orcylaldehyde compound, also can obtain the content of γ-orcylaldehyde compound in cosmetics to cosmetic samples; Detected cosmetic base does not have the restriction of kind, pattern, and it can be white cream, emulsion, aqua cosmetics.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. the present invention provides a kind of method adopting γ-orcylaldehyde compound in liquid chromatographic detection cosmetics first, monitors to cosmetic product quality control and product safety the support that provides the necessary technical, and has positive meaning to the consumption safety of protection cosmetics.
2. the present invention adopts ammonium acetate aqueous solution that testing sample can be made to be uniformly dispersed when sample pre-treatments, be beneficial to follow-up effective extraction, adopt trichloroacetic acid solution-acetonitrile mixed solution as extract, effectively can extract the γ-orcylaldehyde compound in cosmetics, get rid of the interference of all the other components, protein simultaneously in all right deposit sample, extract is clarified, direct examination with computer is got final product after crossing film, and initial strength of mobile phase used in extract and chromatographic resolution is suitable, convenient and swiftly turn avoid because solvent strength does not mate the peak stretching caused; When adopting high performance liquid chromatography to analyze, disengaging time is short, and in sample, impurity is substantially noiseless to target compound, utilizes UV-detector to detect first, and determined wavelength is 280 nm, highly sensitively can detect γ-orcylaldehyde compound.
3. method disclosed by the invention is low to moderate 5 mg/kg to the detection limit of γ-orcylaldehyde compound in cosmetics, and the recovery of standard addition in multiple matrix is all more than 77 %, and relative standard deviation (RSD) is 1.41 ~ 4.63 %; Testing result is accurate, and sample pre-treatments is simple and effective, and analysis time is short, highly sensitive, can meet the requirement of γ-orcylaldehyde compound test in pragmatize cosmetic.
Accompanying drawing explanation
The mutual relationship figure of the concentration-liquid chromatography peak area of the γ-orcylaldehyde that Fig. 1 provides for embodiment one;
The mutual relationship figure of the concentration-liquid chromatography peak area of the chlorination γ-orcylaldehyde that Fig. 2 provides for embodiment one;
The γ-orcylaldehyde compound standard solution liquid chromatographic figure that Fig. 3 provides for embodiment one;
Fig. 4 is the liquid chromatogram of white cream test sample in embodiment two;
Fig. 5 is the liquid chromatogram of emulsion test sample in embodiment two;
Fig. 6 is the liquid chromatogram of aqua test sample in embodiment two;
Fig. 7 is the liquid chromatogram of the white cream test sample of adding γ-orcylaldehyde compound in embodiment three;
Fig. 8 is the liquid chromatogram of the emulsion test sample of adding γ-orcylaldehyde compound in embodiment three;
Fig. 9 is the liquid chromatogram of the aqua test sample of adding γ-orcylaldehyde compound in embodiment three.
Embodiment
Embodiment one sets up γ-orcylaldehyde compound standard curve
50 mg γ-orcylaldehydes (purity >=85%) being dissolved in acetontrile becomes concentration to be the standard reserving solution of 1000 μ g/mL.Pipette Standard Stock solutions acetonitrile-water (75/25, V/V) to be respectively mixed with concentration and to be respectively 0.1,0.2,0.5, the standard working solution of 1.0,5.0,10,50 mg/L totally 7 concentration, get 10 μ L sample introductions to measure by liquid phase chromatogram condition, each serial sample introduction 3 times, is averaged peak area value.
Liquid phase chromatogram condition:
High performance liquid chromatograph, (Agilent 1290, Agilent company of the U.S.);
Chromatographic column: Agilent Eclipse Plus C18,100 × 2.1mm (internal diameter), 1.8 μm (particle diameter);
Mobile phase: A: water; B: acetonitrile;
Type of elution: gradient elution: 0 ~ 8 min, 25 ~ 90 % acetonitriles, 8 ~ 11 min, 90 % acetonitriles, 11 ~ 14 min, 25 % acetonitriles;
Flow velocity: 0.2 mL/min;
UV detect condition: determined wavelength: 280 nm;
Column temperature: 35 DEG C;
Sample size: 10 μ L.
With the peak area of chromatographic peak for ordinate, the γ-orcylaldehyde concentration corresponding with it is horizontal ordinate mapping, and drawing standard working curve, tries to achieve regression equation and be respectively y=65.4 x-3.85.
50 mg chlorination γ-orcylaldehydes (purity >=85%) being dissolved in acetontrile becomes concentration to be the standard reserving solution of 1000 μ g/mL.Pipette Standard Stock solutions acetonitrile-water (75/25, V/V) to be respectively mixed with concentration and to be respectively 0.1,0.2,0.5, the standard working solution of 1.0,5.0,10,50 mg/L totally 7 concentration, get 10 μ L sample introductions to measure by liquid phase chromatogram condition, each serial sample introduction 3 times, is averaged peak area value.
Liquid phase chromatogram condition:
High performance liquid chromatograph, (Agilent 1290, Agilent company of the U.S.);
Chromatographic column: Agilent Eclipse Plus C18,100 × 2.1mm (internal diameter), 1.8 μm (particle diameter);
Mobile phase: A: water; B: acetonitrile;
Type of elution: gradient elution: 0 ~ 8 min, 25 ~ 90 % acetonitriles, 8 ~ 11 min, 90 % acetonitriles, 11 ~ 14 min, 25 % acetonitriles;
Flow velocity: 0.2 mL/min;
UV detect condition: determined wavelength: 280 nm;
Column temperature: 35 DEG C;
Sample size: 10 μ L.
With the peak area of chromatographic peak for ordinate, the chlorination γ-orcylaldehyde concentration corresponding with it is horizontal ordinate mapping, and drawing standard working curve, tries to achieve regression equation and be respectively y=41.4 x-2.58.
As shown in accompanying drawing 1,2, the relation curve of the peak area detected for UV-detector and γ-orcylaldehyde compound concentration, visible, in 0.1 ~ 50 mg/L concentration range, related coefficient between the concentration value of γ-orcylaldehyde compound and response peak area value is respectively 0.999 4 and 0.999 3, in good linear relationship.The detection limit of γ-orcylaldehyde compound is 5 mg/kg, can meet the requirement of cosmetic composition test.
The detection of γ-orcylaldehyde compound in embodiment two cosmetics
(1) sample pretreating
Take sample to be tested 0.20 g(and be accurate to 0.001 g), be placed in 10 mL plastic centrifuge tubes, add the ammonium acetate aqueous solution of 0.15 mL 0.02 mol/L, vortex 30 s, then add 5% trichloroacetic acid-acetonitrile mixed extract (70:30, V/V) 1.85 mL, ultrasonic extraction 15 min after vortex 60 s, then with centrifugal 10 min of 10000 rpm rotating speed, gets supernatant by 0.22 μm of miillpore filter, obtain extract solution, for subsequent use; Above-mentioned sample to be tested is respectively white cream, emulsion and aqua.
(2) liquid phase chromatogram condition
High performance liquid chromatograph, (Agilent 1290, Agilent company of the U.S.);
Chromatographic column: Agilent Eclipse Plus C18,100 × 2.1mm (internal diameter), 1.8 μm (particle diameter);
Mobile phase: A: water; B: acetonitrile;
Type of elution: gradient elution: 0 ~ 8 min, 25 ~ 90 % acetonitriles, 8 ~ 11 min, 90 % acetonitriles, 11 ~ 14 min, 25 % acetonitriles;
Flow velocity: 0.2 mL/min;
UV detect condition: determined wavelength: 280 nm;
Column temperature: 35 DEG C;
Sample size: 10 μ L.
(3) Specimen Determination
Accurately draw 10 μ L extract solutions with automatic sampler and inject high performance liquid chromatograph, measure by chromatographic condition, the retention time of record chromatographic peak and peak area.
γ-orcylaldehyde compound standard product chromatogram is see shown in accompanying drawing 3, and the appearance time that as can be seen from the figure γ-orcylaldehyde compound γ-orcylaldehyde, chlorination γ-orcylaldehyde standard items detect under 280 nm is 3.50 min and 4.53 min.Accompanying drawing 4 ~ 6 is respectively the chromatogram of white cream, emulsion and the aqua cosmetics detected under 280 nm wavelength, and result shows, and γ-orcylaldehyde compound all do not detected in all cosmetic bases.
Embodiment three adds the detection that concentration is γ-orcylaldehyde compound in the cosmetics of 25mg/kg γ-orcylaldehyde and 25mg/kg chlorination γ-orcylaldehyde
(1) sample pretreating
Using with originate in embodiment two identical white cream, emulsion and aqua as matrix, preparation is the white cream of 25 mg/kg γ-orcylaldehydes and 25mg/kg chlorination γ-orcylaldehyde, emulsion and aqua sample to be tested containing concentration.
Take sample to be tested 0.20 g(and be accurate to 0.001 g), be placed in 10 mL plastic centrifuge tubes, add the ammonium acetate aqueous solution of 0.15 mL 0.02 mol/L, vortex 30 s, then add 5% trichloroacetic acid-acetonitrile mixed extract (70:30, V/V) 1.85 mL, ultrasonic extraction 15 min after vortex 60 s, then with centrifugal 10 min of 10000 rpm rotating speed, gets supernatant by 0.22 μm of miillpore filter, obtain extract solution, for subsequent use.
(2) liquid phase chromatogram condition
High performance liquid chromatograph, (Agilent 1290, Agilent company of the U.S.);
Chromatographic column: Agilent Eclipse Plus C18,100 × 2.1mm (internal diameter), 1.8 μm (particle diameter);
Mobile phase: A: water; B: acetonitrile;
Type of elution: gradient elution: 0 ~ 8 min, 25 ~ 90 % acetonitriles, 8 ~ 11 min, 90 % acetonitriles, 11 ~ 14 min, 25 % acetonitriles;
Flow velocity: 0.2 mL/min;
UV detect condition: determined wavelength: 280 nm;
Column temperature: 35 DEG C;
Sample size: 10 μ L.
(4) Specimen Determination
Accurately draw 10 μ L extract solutions with automatic sampler and inject high performance liquid chromatograph, measure by chromatographic condition, the retention time of record chromatographic peak and peak area.
Accompanying drawing 7 ~ 9 is respectively γ-orcylaldehyde compound and goes out peak situation in above-mentioned white cream, emulsion and the patterned cosmetic of aqua, compare with accompanying drawing 2, result shows, add the cosmetic sample matrix of γ-orcylaldehyde compound, the chromatographic peak of γ-orcylaldehyde (3.50 min place) and chlorination γ-orcylaldehyde (4.53min place) all can be detected.
(5) result calculates
Peak area in sample to be tested liquid chromatogram is brought into the typical curve that embodiment one obtains and draws the mass concentration treating γ-orcylaldehyde compound in sample measuring liquid, then according to γ-orcylaldehyde compounds content in following formulae discovery cosmetics:
In formula:
w(γ-orcylaldehyde or chlorination γ-orcylaldehyde)---γ-orcylaldehyde or chlorination γ-orcylaldehyde massfraction in cosmetics, mg/kg;
c---from the mass concentration treating γ-orcylaldehyde or chlorination γ-orcylaldehyde in sample measuring liquid that typical curve checks in, mg/L;
v---sample constant volume is 2 mL;
m---amount of samples is 0.2g.
As calculated, the actual measured value adding white cream, emulsion and aqua sample to be tested that concentration is 25 mg/kg γ-orcylaldehydes and 25mg/kg chlorination γ-orcylaldehyde is respectively: γ-orcylaldehyde, 22.575 mg/kg, 22.075 mg/kg and 22.300 mg/kg; Chlorination γ-orcylaldehyde, 24.275 mg/kg, 22.575 mg/kg and 24.075 mg/kg.
The detection limit of γ-orcylaldehyde compound, the recovery and precision in embodiment four cosmetics
According to the computing method of mark-on sample 10 times of signal to noise ratio (S/N ratio)s, this method is limited to 5 mg/kg to detecting of γ-orcylaldehyde compound.
Accuracy refers to measured value (mean value) and the degree of closeness of actual value, represents the correctness of analysis result.Adopt standard addition method, the γ-orcylaldehyde compound adding 3 varying level concentration in cosmetics carries out recovery test.The horizontal replication of each mark-on 6 times, makes blank assay simultaneously, is greater than 75 % for standard with the recovery; Precision refers to the measured value degree closer to each other of use method replication same homogeneous samples gained, represents the repeatability of analysis result, and conventional relative standard deviation (RSD) represents.The recovery and precision are see table 1.
The table 1 γ-orcylaldehyde compound recovery and Precision test result (n=6)
Table 1 result shows: in the test of matrix mark-on, the recovery of standard addition in three kinds of cosmetic product matrix is good; Can find out from relative standard deviation experimental data, the experiment collimation for three kinds of different substrates is good.
To sum up, in detection cosmetics provided by the invention γ-orcylaldehyde compounds content method in, sample pre-treatments is simple and efficient, and effectively can extract the γ-orcylaldehyde compound in cosmetics, detection limit is low to moderate 5 mg/kg, and the recovery is all at 75 more than %, and relative deviation is little; Be applicable to the Accurate Determining of γ-orcylaldehyde compounds content in dissimilar cosmetics, thus be that cosmetic product quality control and product safety monitor the support that provides the necessary technical, and then the consumption safety of protection cosmetics.
Claims (9)
1. detect a method for γ-orcylaldehyde compound in cosmetics, it is characterized in that, comprise the steps:
(1) sample to be tested is added in ammonium acetate aqueous solution, add the mixed extract that trichloroacetic acid solution and acetonitrile form after vortex again, then through vortex, ultrasonic extraction, obtain extract;
(2) extract is centrifugal, get supernatant micro-pore-film filtration and obtain extract solution;
(3) using acetonitrile and water as mobile phase, high efficiency liquid phase chromatographic analysis method is utilized to detect described extract solution; UV-detector is adopted to detect when carrying out efficient liquid phase chromatographic analysis.
2. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: described γ-orcylaldehyde compound is γ-orcylaldehyde or chlorination γ-orcylaldehyde.
3. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: in step (1), the concentration of ammonium acetate aqueous solution is 0.02 mol/L; The consumption of corresponding every gram of sample to be tested ammonium acetate aqueous solution is 0.75mL.
4. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: in step (1), the time of vortex first time is 30s; The time of second time vortex is 60s; Ultrasonic extraction time is 15min.
5. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: in the trichloroacetic acid solution of step (1), the massfraction of trichloroacetic acid is 5%.
6. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: in the mixed extract that the trichloroacetic acid solution of step (1) and acetonitrile form, the volume ratio of trichloroacetic acid solution, acetonitrile is 75: 25.
7. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: in step (2), rotating speed time centrifugal is 10000 rpm, and the time is 10 min; The aperture of microporous barrier is 0.22 μm.
8. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: when adopting UV-detector to detect in step (3), determined wavelength is 280 nm.
9. detect the method for γ-orcylaldehyde compound in cosmetics according to claim 1, it is characterized in that: adopt gradient elution during efficient liquid phase chromatographic analysis extract solution in step (3), Gradient program is: 0 ~ 8 min, 25 ~ 90 % acetonitriles; 8 ~ 11 min, 90 % acetonitriles; 11 ~ 14 min, 25 % acetonitriles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109061015A (en) * | 2018-10-30 | 2018-12-21 | 福建中烟工业有限责任公司 | Detect method, kit and its application of γ-orcylaldehyde class compound in tobacco product and/or essence spice for cigarette |
| CN114814053A (en) * | 2022-04-13 | 2022-07-29 | 杭州职业技术学院 | Method for detecting content of chloranil and orcinol sensitized perfume in toy |
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| US6268491B1 (en) * | 1991-10-16 | 2001-07-31 | Immulogic Pharmaceutical Corporation | T cell epitopes of the major allergens from dermatophagoides (house dust mite) |
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| ROSSANA BOSSI ET AL.: "A liquid chromatography-mass spectrometric method for the determination of oak moss allergens atranol and chloroatranol in perfumes", 《J.SEP.SCI.》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109061015A (en) * | 2018-10-30 | 2018-12-21 | 福建中烟工业有限责任公司 | Detect method, kit and its application of γ-orcylaldehyde class compound in tobacco product and/or essence spice for cigarette |
| CN114814053A (en) * | 2022-04-13 | 2022-07-29 | 杭州职业技术学院 | Method for detecting content of chloranil and orcinol sensitized perfume in toy |
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