CN107389831B - Method for rapidly detecting forbidden substance estrone in spray cosmetics - Google Patents
Method for rapidly detecting forbidden substance estrone in spray cosmetics Download PDFInfo
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- CN107389831B CN107389831B CN201710881259.5A CN201710881259A CN107389831B CN 107389831 B CN107389831 B CN 107389831B CN 201710881259 A CN201710881259 A CN 201710881259A CN 107389831 B CN107389831 B CN 107389831B
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Abstract
The invention discloses a method for quickly detecting a forbidden substance estrone in a spray cosmetic, which comprises the following steps: step one, manufacturing an open type double-tee capillary spraying device; step two, the open type double-tee capillary spraying device is arranged at the position 3-4 cm away from the front end of a sample inlet of a mass spectrometer, parameters of the mass spectrometer are set, and an aerosol valve of the sample bottle is pressed to obtain a mass spectrum response signal; and step three, in order to improve the response value of the analyte, introducing a derivatization reagent through a syringe pump, blowing atomized liquid drops by atomized gas, and mixing the atomized liquid drops with the sample in the front end space of the capillary spray tube to improve the mass spectrum response signal of the substance to be detected. The method is simple and rapid, and is suitable for rapid detection of the forbidden substance estrone in the spray cosmetics for rapid field detection.
Description
Technical Field
The invention relates to a detection method of a chemical substance, in particular to a rapid detection method of a forbidden substance estrone in a spray cosmetic.
Background
Spray products are products that are widely used in our lives. The product types are mainly divided into two types: one is an aerodynamic spraying product which is provided with spraying power by gas in a bottle body and is also called an aerosol product, and the other is a spraying product which is provided with power by external force (manual) pressing and is commonly called a pressing spraying product. The product has various types, such as: pesticide for agriculture, forestry and household, hair dyeing spray for hair dyeing, spray cosmetic for personal care, and Chinese medicinal spray for traumatic injury. These products offer convenience in life and are potentially harmful to the human body and the environment. The efficacy of the spray product is mainly achieved because the product contains specific chemical functional components. However, in order to increase its efficacy, an illegal merchant may illegally add some prohibited substances having the same efficacy. In the using process, because the inferior products contain toxic and harmful substances, the toxic and harmful substances can enter human bodies through skin contact, eye contact, inhalation and other modes, and symptoms such as dizziness, nausea, vomiting, allergy and the like are caused, so that the inferior products are seriously dangerous to human health. In China, technical Specifications for cosmetic safety (2015 edition) and European Union cosmetic laws (EC 1223/2009) definitely stipulate estrone as a forbidden substance in cosmetics.
Disclosure of Invention
The invention aims to provide a method for banning estrone in a spray cosmetic, which is convenient, efficient and suitable for on-site rapid detection.
A method for rapidly detecting a forbidden substance estrone in a spray cosmetic comprises the following steps:
step one, manufacturing an open type double-tee capillary spraying device;
the open type double-tee capillary spraying device comprises a first three-way pipe and a second three-way pipe which are connected in series, a sample channel is formed in the horizontal direction, a capillary spraying pipe is arranged on the sample channel, the rear end of the capillary spraying pipe is connected with one end of a flow dividing pipe, the front end of the capillary spraying pipe is arranged in the sample channel, the capillary spraying pipe is close to the right end of the second three-way pipe, a mixing space is formed between the capillary spraying pipe and the right end of the second three-way pipe, the other end of the flow dividing pipe is respectively connected with a sample bottle and a waste liquid bottle through a pipeline, the first three-way pipe is connected with a gas supply device through a pipeline, the second three-way pipe is connected with an injection pump through a pipeline, and a mass;
step two, the open type double-tee capillary spraying device is arranged at the position 3-4 cm away from the front end of a sample inlet of a mass spectrometer, and the parameters of the mass spectrometer are set as follows: positive ion mode, capillary voltage 4 kV; setting the gas pressure of the gas supply device to 30 psi; pressing an aerosol valve of the sample bottle to obtain a mass spectrum response signal;
step three, improving the response value of the analyte
The injection pump introduces liquid, the propelling speed is 20 mu L/min, atomized liquid drops are blown away by atomized gas, the atomized liquid drops are mixed with a sample in the front end space of the capillary spray tube, and the mass spectrum response signal of a substance to be detected is improved.
The invention relates to a method for rapidly detecting a forbidden substance estrone in a spray cosmetic, wherein a spray sample is the spray cosmetic.
The invention relates to a method for rapidly detecting a forbidden substance estrone in a spray cosmetic, wherein mass spectrum information of a substance to be detected is shown in a table 1.
TABLE 1 Mass Spectrometry information of the test substances
The invention relates to a method for rapidly detecting forbidden substance estrone in spray cosmetics, wherein a first three-way pipe and a second three-way pipe respectively comprise a horizontal pipe and a vertical pipe, the left end of the horizontal pipe of the first three-way pipe is sealed by a fixing piece, the right end of the horizontal pipe of the second three-way pipe is connected with the left end of the horizontal pipe of the second three-way pipe, a through hole is formed in the fixing piece, and the rear end of a capillary spray pipe penetrates out of the through hole and is connected with a shunt pipe.
The invention relates to a method for rapidly detecting a forbidden substance estrone in a spray cosmetic, wherein a vertical pipe of a first three-way pipe is connected with a gas supply device through a pipeline, and a vertical pipe of a second three-way pipe is connected with an injection pump through a pipeline.
The invention relates to a method for rapidly detecting a forbidden substance estrone in spray cosmetics, wherein the joints of a first three-way pipe and a second three-way pipe are 1/8 inches or 1/16 inches; the inner diameter of the capillary spraying pipe is 10-200 mu m.
The method for rapidly detecting the forbidden substance estrone in the spray cosmetics comprises the steps that the front end of the capillary spraying pipe is arranged in the second three-way pipe, and the distance between the front end of the capillary spraying pipe and the right end of the horizontal pipe of the second three-way pipe is 1-3 cm.
The invention relates to a method for quickly detecting a forbidden substance estrone in a spray cosmetic, wherein a flow regulating valve is arranged on a shunt pipe.
The invention relates to a method for rapidly detecting a forbidden substance estrone in a spray cosmetic, wherein liquid introduced by a syringe pump is a methoxylamine derivatization reagent.
The method for quickly detecting the forbidden substance estrone in the spray cosmetics is different from the prior art in that:
the invention relates to a rapid detection method for a forbidden substance estrone in a spray cosmetic, which establishes a detection method for rapidly screening the forbidden substance estrone in the spray cosmetic by a double-tee capillary spray tandem ion trap mass spectrum.
The invention discloses a method for quickly detecting the forbidden substance estrone in the spray cosmetics, which has the innovativeness and advantages that:
1. the invention provides a method for a double-tee-joint capillary spray tandem mass spectrum for the first time, which is used for rapidly detecting the forbidden substance estrone in the spray cosmetics.
2. The invention is suitable for the detection method for detecting the forbidden substances of the spray products by adopting the double-tee capillary spray tandem mass spectrum, and the response value of the estrone is improved by introducing a derivatization reagent, and the detection limit of the estrone is 50 mu g/kg.
3. The invention does not need to use an extraction solvent.
The method for rapidly detecting the forbidden substance estrone in the spray cosmetic of the present invention is further described with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic structural view of an open-type double-tee capillary spray device according to the present invention;
FIG. 2 is a mass spectrum of estrone in a cosmetic spray product according to the method of the present invention;
all english-chinese references appearing in the drawings accompanying the description of the invention are as follows:
m/z: a mass to nuclear ratio; relative arrival: relative abundance; intensity: strength; estrone: estrone.
Detailed Description
A first tee and a second tee (shivialock (shanghai) fluid systems technologies ltd); microelectrode drawing machine model P-1000 (Sutter, USA); capillary spray tubes (Feng chromatographic devices, Inc. Yongnian); BrukeramaZon ion trap mass spectrometer (Bruker Dalton, USA).
A method for rapidly detecting a forbidden substance estrone in a spray cosmetic comprises the following steps:
step one, manufacturing an open type double-tee capillary spraying device;
as shown in fig. 1, the open-type double-tee capillary spraying device comprises a first three-way pipe 1 and a second three-way pipe 2 which are connected in series, a sample channel is formed in the horizontal direction, a capillary spraying pipe 3 is arranged on the sample channel, the rear end of the capillary spraying pipe 3 is connected with one end of a shunt pipe 4, the front end of the capillary spraying pipe is arranged in the sample channel, a mixing space is formed between the capillary spraying pipe and the right end of the second three-way pipe 2 close to the right end of the second three-way pipe 2, the other end of the shunt pipe 4 is respectively connected with a sample bottle 5 and a waste liquid bottle 6 through pipelines, the first three-way pipe 1 is connected with a gas supply device 7 through a pipeline, the second three-way pipe 2 is connected with an injection pump 8 through a pipeline, and;
the following is the preferred technical scheme of the open type double-tee capillary spraying device:
first three-way pipe 1 and second three-way pipe 2 all include horizontal pipe and vertical pipe, and the left end of the horizontal pipe of first three-way pipe 1 adopts stationary blade 10 to seal, and the right-hand member links to each other with the left end of the horizontal pipe of second three-way pipe 2, is provided with the through-hole on stationary blade 10, and the rear end of capillary spraying pipe 3 is worn out from the through-hole, links to each other with shunt tubes 4.
The vertical pipe of the first three-way pipe 1 is connected with the gas supply device 7 through a pipeline, and the vertical pipe of the second three-way pipe 2 is connected with the injection pump 8 through a pipeline.
The interface of the first tee 1 and the second tee 2 is 1/8 inches or 1/16 inches; the inner diameter of the capillary spray tube 3 is 10 to 200 μm.
The front end of the capillary spraying pipe 3 is arranged in the second three-way pipe 2, and the distance between the front end of the capillary spraying pipe 3 and the right end of the horizontal pipe of the second three-way pipe 2 is 1-3 cm.
A flow regulating valve is arranged on the shunt pipe 4.
Step two, the open-type double-tee capillary tube spraying device is arranged at the front end of a sample inlet of the mass spectrometer 9 by 3-4 cm, and the parameters of the mass spectrometer 9 are set as follows: positive ion mode, capillary voltage 4 kV; setting the gas pressure of the gas supply device 7 to 30 psi; pressing an aerosol valve of the sample bottle 5 to obtain a mass spectrum response signal;
step three, improving the response value of the analyte
The injection pump 8 introduces liquid with the propelling speed of 20 mu L/min, atomized liquid drops are blown away by atomized gas and mixed with the sample in the front end space of the capillary spray tube 3, and the mass spectrum response signal of the substance to be detected is improved.
The spray sample in sample bottle 5 is a spray cosmetic sample.
The mass spectrum information of the test substance is shown in table 1.
TABLE 1 Mass Spectrometry information of the test substances
The liquid introduced by the injection pump 8 is a methoxyamine derivatization reagent.
The chemical information of the substances to be tested is shown in table 2:
TABLE 2 chemical information of the substances to be tested
The mass spectrum is shown in FIG. 2.
The analyte analysis conditions involved in the present invention are all positive ion modes, and usually a derivatization reagent is introduced to improve the response value of the analyte. This patent relates to such a method of improving response values.
One path of the double-tee capillary spraying device introduces atomizing gas, and the other path introduces derivatization reagent methoxylamine. Through determination, the response value of estrone in the spray cosmetic is obviously improved through derivatization reaction. The detection limit of estrone is determined to be 50 mug/kg by detection with about 3 times signal to noise ratio.
The specific detection method comprises the following steps:
firstly, the rapid detection of estrone in the spray cosmetics.
The first step is as follows: manufacturing an open type double-tee capillary spraying device;
the second step is that: : and (3) preparing a positive sample, namely adding estrone standard solutions with different concentrations into the spray cosmetic water which does not contain estrone through detection to prepare the positive sample.
The quick detection method of the double-tee capillary comprises the following steps: and connecting the positive spray toning lotion sample with an open type double-tee capillary spraying device. The inner diameter of the capillary spray tube 3 is 20 μm, the distance from the sample inlet of the mass spectrometer 9 is 3cm, and the air pressure is 30 psi. The mass spectrometry conditions were set as follows: positive ion mode, capillary voltage 4 kV. And pressing the product aerosol valve to obtain a mass spectrum response signal.
The third step: increasing the response value of an analyte
The injection pump 8 introduces a methoxyamine derivatization reagent of 100mM, the propelling speed is 20 muL/min, atomized methoxyamine droplets are blown away by atomizing gas, derivatization reaction is carried out in the front end space of the capillary spray tube 3, the mass spectrum response signal of the estrone is improved, and the mass spectrum after derivatization is shown in figure 2.
Before derivatization, the parent ion of estrone is m/z 271.3, which is greatly interfered by noise and has low response value. Through the device, a methoxyamine derivatization reagent is introduced, the selection of a monitoring parent ion of estrone is m/z 300.2, the selection of a corresponding daughter ion is m/z252.8, and the response value is obviously improved by 24 times compared with that of underivation.
The above specific applications are exemplary only, and not limiting, and all parameter selections within the scope of the invention yield similar results.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (7)
1. A method for rapidly detecting a forbidden substance estrone in a spray cosmetic is characterized by comprising the following steps: the method comprises the following steps:
step one, manufacturing an open type double-tee capillary spraying device;
the open type double-tee capillary spraying device comprises a first tee pipe (1) and a second tee pipe (2) which are connected in series, a sample channel is formed in the horizontal direction, a capillary spray tube (3) is arranged on the sample channel, the rear end of the capillary spray pipe (3) is connected with one end of a shunt pipe (4), the front end is arranged in the sample channel and is close to the right end of the second three-way pipe (2), a mixing space is formed between the two ends of the two-way pipe (2) and the other end of the shunt pipe (4) is respectively connected with a sample bottle (5) and a waste liquid bottle (6) through pipelines, the first three-way pipe (1) is connected with a gas supply device (7) through a pipeline, the second three-way pipe (2) is connected with an injection pump (8) through a pipeline, a mass spectrometer (9) is arranged on the right side of the second three-way pipe (2);
step two, the open type double-tee capillary spraying device is arranged at the position 3-4 cm away from the front end of a sample inlet of a mass spectrometer (9), and the parameters of the mass spectrometer (9) are set as follows: positive ion mode, capillary voltage 4 kV; setting the gas pressure of the gas supply device (7) to 30 psi; pressing an aerosol valve of the sample bottle (5) to obtain a mass spectrum response signal;
step three, improving the response value of the analyte:
the injection pump (8) introduces liquid, the propelling speed is 20 mu L/min, atomized liquid drops are blown away by atomized gas and are mixed with a sample in the front end space of the capillary spray tube (3), and the mass spectrum response signal of a substance to be detected is improved;
the liquid introduced by the injection pump (8) is a methoxylamine derivatization reagent.
2. The method for rapidly detecting estrone as a banned substance in a spray cosmetic composition according to claim 1, wherein:
TABLE 1 Mass Spectrometry information of the test substances
The mass spectrum information of the test substance is shown in table 1.
3. The method for rapidly detecting the banned substance estrone in a spray cosmetic as claimed in claim 2, wherein: the first three-way pipe (1) and the second three-way pipe (2) both comprise a horizontal pipe and a vertical pipe, the left end of the horizontal pipe of the first three-way pipe (1) is sealed by a fixing piece (10), the right end of the horizontal pipe of the second three-way pipe (2) is connected with the left end of the horizontal pipe of the second three-way pipe, a through hole is formed in the fixing piece (10), and the rear end of the capillary spraying pipe (3) penetrates out of the through hole and is connected with the flow dividing pipe (4).
4. The method for rapidly detecting the banned substance estrone in a spray cosmetic as claimed in claim 3, wherein: the vertical pipe of the first three-way pipe (1) is connected with the gas supply device (7) through a pipeline, and the vertical pipe of the second three-way pipe (2) is connected with the injection pump (8) through a pipeline.
5. The method for rapidly detecting the banned substance estrone in a spray cosmetic as claimed in claim 4, wherein: the interface of the first tee (1) and the second tee (2) is 1/8 inches or 1/16 inches; the inner diameter of the capillary spraying pipe (3) is 10-200 mu m.
6. The method for rapidly detecting estrone as a banned substance in a spray cosmetic composition according to claim 5, wherein: the front end of the capillary spraying pipe (3) is arranged in the second three-way pipe (2), and the distance between the front end of the capillary spraying pipe and the right end of the horizontal pipe of the second three-way pipe (2) is 1-3 cm.
7. The method for rapidly detecting estrone as a banned substance in a spray cosmetic composition according to claim 6, wherein: and a flow regulating valve is arranged on the shunt pipe (4).
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| CN201710881259.5A CN107389831B (en) | 2017-09-26 | 2017-09-26 | Method for rapidly detecting forbidden substance estrone in spray cosmetics |
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| CN107389831B true CN107389831B (en) | 2020-01-21 |
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| CN117871742B (en) * | 2023-05-30 | 2024-09-17 | 广东新征程生命科学有限公司 | Device and method for preparing detection sample solution for measuring estrogen content |
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