CN114814053A - Method for detecting content of chloranil and orcinol sensitized perfume in toy - Google Patents
Method for detecting content of chloranil and orcinol sensitized perfume in toy Download PDFInfo
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- CN114814053A CN114814053A CN202210386295.5A CN202210386295A CN114814053A CN 114814053 A CN114814053 A CN 114814053A CN 202210386295 A CN202210386295 A CN 202210386295A CN 114814053 A CN114814053 A CN 114814053A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a method for detecting the content of chloranil and orcinol sensitizing perfume in a toy, which comprises the following steps: the method comprises the following steps: preparing a series of standard solutions of chloranil and orcinol, measuring by using a gas chromatography-mass spectrometer, and drawing a standard curve fit by using the mass concentration of the standard solution and the corresponding peak area to obtain a linear regression equation; step two: carrying out ultrasonic extraction on a toy sample for testing to obtain a liquid to be tested; step three: and (3) detecting the liquid to be detected by using a gas chromatography-mass spectrometer, and substituting the detected peak area into the regression equation in the step (1) to obtain the content of chloranilol and orcinol in the sample. The method provided by the invention is simple and convenient to operate, low in detection limit and high in precision, is suitable for the determination of the content of the sensitization spices chloranil and orcinol in the field, and has important significance for protecting the rights of consumers of children and promoting the smooth export of toy products. Besides, the method also has the advantages of simple operation, high accuracy and good reproducibility.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a method for detecting the content of chloranilol and orcinol sensitizing perfume in a toy.
Background
In the production process of some children toys, in order to increase the attraction to children or cover up unpleasant odor contained in the toys, some essence and spice are often added to make the toys fragrant. Among these mixed perfumes, those having a certain sensitizing property are called sensitizing perfumes. The chemical components of the fragrance can be absorbed into the human body through the mouth, nose and skin, and the components can reach all parts of the body through the blood circulation.
Relevant studies have shown that at least 1% to 2% of people develop allergic symptoms after exposure to a fragrance. Allergic fragrances have been reported to be one of the most prominent sources of contact injury in children's life.
However, at present, no method for detecting the content of chloranilol and orcinol sensitized aromatics in toys at home and abroad exists, and no relevant literature report on the detection of chloranilol and orcinol is found yet.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides the detection method of the chloranilol and orcinol sensitized perfume in the toy, which has the advantages of high accuracy and good reproducibility.
A method of detecting chloranil and orcinol sensitising fragrance content in a toy, comprising the steps of:
the method comprises the following steps: preparing a series of standard solutions of chloranil and orcinol, measuring by using a gas chromatography-mass spectrometer, and drawing a standard curve fit by using the mass concentration of the standard solution and the corresponding peak area to obtain a linear regression equation;
step two: processing the toy sample for testing to obtain a liquid to be tested;
step three: detecting the liquid to be detected by using gas chromatography-mass spectrometry, and substituting the measured peak area into the regression equation in the step (1) to obtain the mass concentrations of chloranilol and orcinol in the sample;
the gas chromatography-mass spectrometry detection conditions are as follows: adopting a DB-5MS chromatographic column, and carrying out temperature programming: keeping the temperature at 100 ℃ for 1min, heating to 200 ℃ at 10 ℃/min, then heating to 260 ℃ at 30 ℃/min, and keeping the temperature for 2 min; carrier gas: helium with purity not lower than 99.999%; flow rate: 1.0 mL/min; sample inlet temperature: 220 ℃; transmission line temperature: 260 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 1 mu L of the solution; an ionization mode: an EI source; ionization energy: 70 eV; the scanning mode is as follows: full scan and selective ion scan combined mode, solvent delay: 3 min.
Further, the method for detecting the content of chloranilol and orcinol sensitizing fragrance in a toy as described above, the first step comprising:
step 11: accurately weighing chloranil alcohol and orcinol standard substances respectively, and preparing a standard stock solution with the mass concentration of 1000mg/L by using a mixed solution of methanol and dichloromethane in a volume ratio of 1: 1;
step 12: respectively transferring the standard stock solutions into volumetric flasks of 10.0mL to 100mL respectively, carrying out constant volume to scale with a mixed solution of methanol and dichloromethane in a volume ratio of 1:1, shaking up, and preparing into a mixed standard stock solution with a mass concentration of 100 mg/L;
step 13: gradually diluting the mixed standard stock solution to a standard solution with a series of concentrations of (1.0, 2.0, 5.0, 10, 20, 100) mg/L by using a mixed solution of methanol and dichloromethane with a volume ratio of 1: 1;
step 14: and performing linear regression by taking the peak area as a vertical coordinate and the mass concentration in the standard solution as a horizontal coordinate to obtain regression equations of chloranilol and orcinol.
Further, the method for detecting the content of chloranilol and orcinol sensitizing fragrance in a toy as described above, wherein the second step comprises:
accurately weighing 0.5g of toy sample for test in a glass sample bottle, adding 10.00mL of mixed solution of methanol and dichloromethane with the volume ratio of 1:1, sealing, placing in an ultrasonic extractor for ultrasonically extracting chloranil and orcinol in the toy, cooling the glass sample bottle containing the sample to normal temperature, and allowing an extracting solution to pass through a sample filter for testing.
Further, the method for detecting the content of chloranil and orcinol sensitized perfumes in the toys as described above, wherein the ultrasonic extraction time is (30 +/-5) min.
Further, according to the method for detecting the content of the chloranilol and orcinol sensitized perfume in the toy, if the extracting solution is rich in impurities, the extracting solution is centrifuged at 10000r/min for 10min, the supernatant is taken and filtered by a sample filter, and the filtrate is used as the solution to be detected.
Has the advantages that:
the invention adopts methanol and dichloromethane (volume ratio is 1:1) as extraction solvent, and the extraction solvent is subjected to ultrasonic extraction, volume fixing and filtration, and then the measurement is carried out by means of a gas chromatography-mass spectrometer, wherein the instrument conditions are as follows: column DB-5MS (30 m.times.0.25 mm. times.0.25 μm), temperature programmed: maintaining at 100 deg.C for 1min, heating to 200 deg.C at 10 deg.C/min, heating to 260 deg.C at 30 deg.C/min, and maintaining for 2 min; carrier gas: helium with purity not lower than 99.999%; flow rate: 1.0 mL/min; sample inlet temperature: 220 ℃; transmission line temperature: 260 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 1 mu L of the solution; an ionization mode: an EI source; ionization energy: 70 eV; the scanning mode is as follows: full scan and selective ion Scan (SIM) combined mode, solvent delay: 3min, the detection limit of the method can reach 2.0 mg/kg.
The method provided by the invention solves the problem that no method for specially detecting chloranil and orcinol exists in the field at home and abroad, is simple and convenient to operate, low in detection limit and high in precision, is suitable for the determination of the content of the forbidden sensitizing spices chloranil and orcinol in the field, and has important significance for improving the quality level of toys in China, protecting the rights and interests of consumers of children and promoting the smooth export of the toy products. Besides, the method also has the advantages of simple operation, high accuracy and good reproducibility.
Drawings
FIG. 1 is a chromatogram of chloranilol and orcinol;
figure 2 is a mass spectrum of chloranil;
FIG. 3 is a mass spectrum of orcinol.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Instruments and reagents:
7890B/5975C GC-MS with EI ionization source, Agilent instruments, Inc., USA; ultrasonic cleaners (Branson Corp); one in ten thousand electronic analytical balance (beijing sidoris ltd); chloranil and orcinol (purity greater than 98%) germany dr. ehrenstorfer company; methanol and dichloromethane (chromatographically pure, Fisher company).
The method for detecting the content of chloranilol and orcinol in the toy provided by the embodiment comprises the following steps:
(1) preparing standard solution and fitting standard curve equation
Accurately weighing chloranil alcohol and orcinol standard substances (the purity is more than 98 percent) respectively, and preparing standard stock solutions with the mass concentration of 1000mg/L by using methanol and dichloromethane (the volume ratio is 1: 1);
respectively transferring the standard stock solutions into volumetric flasks of 10.0mL to 100mL respectively, carrying out constant volume to scale with a solution of methanol and dichloromethane (volume ratio is 1:1), shaking up, and preparing a mixed standard stock solution with the mass concentration of 100 mg/L;
then gradually diluting the solution with methanol and dichloromethane (volume ratio is 1:1) to standard solution with mass concentration of (1.0, 2.0, 5.0, 10, 20, 100) mg/L series concentration;
performing linear regression by taking the peak area as a vertical coordinate (Y) and the mass concentration in the standard solution as a horizontal coordinate (X) to obtain a regression equation of chloranilol and orcinol;
(2) sample processing
Accurately weighing 0.5g (accurate to 1mg) of sample (toy for test) in a glass sample bottle, adding 10.00mL of methanol and dichloromethane (volume ratio is 1:1) solution, sealing, placing in an ultrasonic extractor, performing ultrasonic extraction (30 +/-5) min to remove chloranil and orcinol in the toy, cooling the glass sample bottle containing the sample to normal temperature, and allowing the extract to pass through a sample filter for testing. And if the extracting solution contains more impurities, centrifuging at 10000r/min for 10min, taking supernatant, filtering by a sample filter, and taking filtrate as the solution to be detected.
(3) Gas chromatography-mass spectrometry detection
Adopting a DB-5MS chromatographic column, and carrying out temperature programming: keeping the temperature at 100 ℃ for 1min, heating to 200 ℃ at 10 ℃/min, then heating to 260 ℃ at 30 ℃/min, and keeping the temperature for 2 min; carrier gas: helium with purity not lower than 99.999%; flow rate: 1.0 mL/min; sample inlet temperature: 220 ℃; transmission line temperature: 260 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 1 mu L of the solution; an ionization mode: an EI source; ionization energy: 70 eV; the scanning mode is as follows: full scan and selective ion Scan (SIM) combined mode, solvent delay: and (3) detecting by using a gas chromatography-mass spectrometer, and substituting the measured peak areas into the regression equation in the step (1) to obtain the mass concentrations of chloranilol and orcinol in the sample.
According to the detection method provided by the invention, the peak area and the mass concentration have a good linear relation within the range of (1.000-100) mg/L, and the correlation coefficient is 0.9991. The standard recovery rates of different levels of high, medium and low are 82.3% -102.8%, and the relative standard deviation (namely precision) is 1.8% -8.2%.
FIG. 1 is a chromatogram of chloranilol and orcinol; figure 2 is a mass spectrum of chloranil; FIG. 3 is a mass spectrum of orcinol; through the drawings of fig. 1-3, the method is accurate and reliable, and can meet the detection requirements of chloranilol and orcinol in toys.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A method for detecting the content of chloranilol and orcinol sensitizing fragrance in a toy, comprising the steps of:
the method comprises the following steps: preparing a series of standard solutions of chloranil and orcinol, measuring by using a gas chromatography-mass spectrometer, and drawing a standard curve fit by using the mass concentration of the standard solution and the corresponding peak area to obtain a linear regression equation;
step two: carrying out pretreatment on a toy sample for testing to obtain a liquid to be tested;
step three: detecting the liquid to be detected by using a gas chromatography-mass spectrometer, substituting the detected peak area into the regression equation in the step (1) to obtain the mass concentrations of chloranilol and orcinol in the sample;
the gas chromatography-mass spectrometry detection conditions are as follows: adopting a DB-5MS chromatographic column, and carrying out temperature programming: keeping the temperature at 100 ℃ for 1min, heating to 200 ℃ at 10 ℃/min, then heating to 260 ℃ at 30 ℃/min, and keeping the temperature for 2 min; carrier gas: helium with purity not lower than 99.999%; flow rate: 1.0 mL/min; sample inlet temperature: 220 ℃; transmission line temperature: 260 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 1 mu L of the solution; an ionization mode: an EI source; ionization energy: 70 eV; the scanning mode is as follows: full scan and selective ion scan combined mode, solvent delay: 3 min.
2. The method of claim 1, wherein the first step comprises:
step 11: accurately weighing chloranil alcohol and orcinol standard substances respectively, and preparing a standard stock solution with the mass concentration of 1000mg/L by using a mixed solution of methanol and dichloromethane in a volume ratio of 1: 1;
step 12: respectively transferring the standard stock solutions into volumetric flasks of 10.0mL to 100mL respectively, carrying out constant volume to scale with a mixed solution of methanol and dichloromethane in a volume ratio of 1:1, shaking up, and preparing into a mixed standard stock solution with a mass concentration of 100 mg/L;
step 13: gradually diluting the mixed standard stock solution to a standard solution with a series of concentrations of 1.0, 2.0, 5.0, 10, 20 and 100mg/L by using a mixed solution of methanol and dichloromethane in a volume ratio of 1: 1;
step 14: and performing linear regression by taking the peak area as a vertical coordinate and the mass concentration in the standard solution as a horizontal coordinate to obtain regression equations of chloranilol and orcinol.
3. The method of claim 1, wherein the second step comprises:
accurately weighing 0.5g of toy sample for test in a glass sample bottle, adding 10.00mL of mixed solution of methanol and dichloromethane with the volume ratio of 1:1, sealing, placing in an ultrasonic extractor for ultrasonically extracting chloranil and orcinol in the toy, cooling the glass sample bottle containing the sample to normal temperature, and allowing an extracting solution to pass through a sample filter for testing.
4. The method of detecting the amount of chloranilol and orcinol-sensitizing fragrance in a toy according to claim 3, wherein the time period for the ultrasonic extraction is 30 ± 5 min.
5. The method for detecting the content of chloranilol and orcinol-sensitized perfume in a toy according to claim 3, wherein if the extract contains more impurities, the extract is centrifuged at 10000r/min for 10min, and the supernatant is filtered by a sample filter to obtain a filtrate as a solution to be detected.
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| CN202210386295.5A CN114814053A (en) | 2022-04-13 | 2022-04-13 | Method for detecting content of chloranil and orcinol sensitized perfume in toy |
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| CN202210386295.5A CN114814053A (en) | 2022-04-13 | 2022-04-13 | Method for detecting content of chloranil and orcinol sensitized perfume in toy |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104764817A (en) * | 2015-03-19 | 2015-07-08 | 苏州出入境检验检疫局检验检疫综合技术中心 | Method for detecting atranol compound in cosmetic |
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- 2022-04-13 CN CN202210386295.5A patent/CN114814053A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104764817A (en) * | 2015-03-19 | 2015-07-08 | 苏州出入境检验检疫局检验检疫综合技术中心 | Method for detecting atranol compound in cosmetic |
Non-Patent Citations (2)
| Title |
|---|
| AMAR G. CHITTIBOYINA等: "Chromatographic analyses and unambiguous identification of atranol-like secondary metabolites in oakmoss absolute", 《FLAVOUR FRAGR J.》 * |
| CRISTINA AVONTO等: "Are atranols the only skin sensitizers in oakmoss? A systematic investigation using non-animal methods", 《TOXICOLOGY IN VITRO》 * |
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