CN111855866A - Method for rapidly determining formaldehyde in tobacco additive - Google Patents
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- CN111855866A CN111855866A CN202010860718.3A CN202010860718A CN111855866A CN 111855866 A CN111855866 A CN 111855866A CN 202010860718 A CN202010860718 A CN 202010860718A CN 111855866 A CN111855866 A CN 111855866A
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Abstract
The invention belongs to the technical field of physical and chemical inspection of tobacco additives, and particularly relates to a detection method for rapidly determining formaldehyde in a tobacco additive; the method comprises the following steps: (1) preparing a standard working solution; (2) preparing a derivatization reagent; (3) preparing an extraction solution; (4) preparing a sample solution; (5) blank test; (6) ultra-high performance liquid chromatography analysis: respectively detecting and analyzing the standard working solution, the sample solution and the blank test solution with 6 concentration levels by using an ultra-high performance liquid chromatograph; (7) establishing a standard working curve; (8) calculating a result; the invention prepares a series of low-concentration standard working solutions, so that the concentration of formaldehyde in the additive used by the company falls within the range of a standard working curve, thereby improving the accuracy of data; the detection method is simple, convenient and accurate, and has good repeatability and high sensitivity; and the detection method greatly shortens the analysis time, reduces the loss of the mobile phase and reduces the pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of physical and chemical inspection of tobacco additives, and particularly relates to a detection method for rapidly determining formaldehyde in a tobacco additive.
Background
The additive for cigarette is an important raw material added for improving the smoking quality of cigarette, has certain fragrance, can play the roles of adding fragrance and correcting taste, adjusting the smoke smell, supplementing the smoke smell and covering miscellaneous gas in various tobacco products, can enable the cigarette to generate better smoke effect during smoking, and has the safety directly influencing the quality safety of the cigarette products.
In the tobacco industry, 6 additives such as formaldehyde and the like are mainly monitored in 2011, and 16 additives such as formaldehyde and the like are forbidden to be used in the research on the permission and the corresponding limitation of the additives for cigarettes. The harm of formaldehyde to human body is mainly manifested by stimulation, carcinogenesis and mutagenic effect, which can stimulate respiratory system of human body to different extent in the process of cigarette smoking, and can cause harm to human body after long-term inhalation.
At present, the detection technology of formaldehyde comprises a spectrophotometry method, an electrochemical method, a chromatography method and a sensor method, the tobacco additive sample matrix is generally complex, the interference is more, the formaldehyde content is low, the Ultra Performance Liquid Chromatography (UPLC) has high sensitivity, accurate quantification and strong anti-interference performance, and the measurement of the formaldehyde in the tobacco additive is not reported. Meanwhile, the concentration of formaldehyde in the tobacco additive used by the company is far lower than the lowest standard solution concentration of 0.109mg/L in YC/T359-2010 high performance liquid chromatography for measuring formaldehyde in the tobacco additive, and the detection time of the standard method is about 20 minutes, so that an analysis method for quickly measuring formaldehyde in the tobacco additive is urgently needed to be established based on the prior art.
Disclosure of Invention
The invention aims to prepare a series of low-concentration standard working solutions based on the prior art, and establish an analysis method for rapidly and efficiently determining formaldehyde in a cigarette additive by using UPLC (ultra performance liquid chromatography) so as to improve the safety of cigarette products; the method is not reported in documents, the pretreatment is simple, the formaldehyde content in the tobacco additive can be rapidly, efficiently and economically determined, the efficiency of detecting the formaldehyde in the tobacco additive is improved, the analysis time is greatly shortened, the loss of a mobile phase is reduced, and the pollution to the environment is reduced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for rapidly determining formaldehyde in a tobacco additive comprises the following steps of extracting formaldehyde in the additive by using an extraction solution, carrying out derivatization treatment, and analyzing the formaldehyde in the tobacco additive by using an ultra-high performance liquid chromatography isocratic elution method:
(1) preparation of standard working solutions: preparing 6-grade standard working solution with concentration gradient, which contains formaldehyde-2, 4-dinitrophenylhydrazone;
(2) preparation of derivatization reagent: weighing 2, 4-dinitrophenylhydrazine in a brown volumetric flask, adding phosphoric acid, and diluting to the constant volume with acetonitrile to prepare a 2, 4-dinitrophenylhydrazine acetonitrile phosphoric acid solution;
(3) preparation of extraction solution: preparing tetrahydrofuran-water solution;
(4) preparation of sample solution: weighing 1g, accurately measuring to 0.1mg, placing a sample in a 50mL conical flask with a plug, adding 20.00mL of extraction solution, fully and uniformly mixing, placing in a rotary oscillator, rotationally oscillating at 100rpm for 5min, standing for 1min, accurately transferring 1mL of supernatant into a 10mL volumetric flask, accurately transferring 1mL of derivatization reagent, fixing the volume of the extraction solution, placing for 10min for derivatization, filtering with a 0.22 mu m organic filter membrane, and obtaining a filtrate which is a sample solution;
(5) blank test: repeating the rest steps in the step (4) without adding a sample;
(6) ultra-high performance liquid chromatography analysis: respectively detecting and analyzing the standard working solution, the sample solution and the blank test solution with 6 concentration levels by using an ultra-high performance liquid chromatograph;
(7) establishing a standard working curve: converting formaldehyde-2, 4-dinitrophenylhydrazone into formaldehyde concentration, and establishing a working curve of the standard working solution by using a peak area which is equivalent to the area where the equivalent concentration of the formaldehyde corresponds to the formaldehyde-2, 4-dinitrophenylhydrazone in the standard working solution;
(8) and (4) calculating a result: substituting the chromatographic peak area of the formaldehyde-2, 4-dinitrophenylhydrazone of the sample solution measured under the same condition into the standard working curve obtained in the step (7) to obtain the concentration of the formaldehyde, thereby obtaining the content of the formaldehyde in the additive sample.
Further, the specific preparation method of the standard working solution in the step (1) is that 0.5mL1.0mg/mL formaldehyde-2, 4-dinitrophenylhydrazone is accurately transferred into a 50mL volumetric flask by a pipette, and acetonitrile is subjected to constant volume to be determined as a level 1 standard solution; adding 20.00mL of the 1 st-grade standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 2 nd-grade standard solution; adding 20.00mL of the grade 2 standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a grade 3 standard solution; adding 20.00mL of the 3 rd-level standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to be determined as a 4 th-level standard solution; adding 20.00mL of the 4 th-level standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 5 th-level standard solution; and (3) adding 20.00mL of the 5 th-grade standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 6 th-grade standard solution.
Further, in the preparation step (2), 0.1g of 2, 4-dinitrophenylhydrazine is weighed in a 100mL brown volumetric flask, 0.5mL of phosphoric acid is added, and acetonitrile is used for constant volume to prepare a 2, 4-dinitrophenylhydrazine acetonitrile phosphoric acid solution with the concentration of 1.0mg/mL of 2, 4-dinitrophenylhydrazine.
Further, in the step (3), tetrahydrofuran: the volume ratio of water was 9: 1.
Further, the specific conditions of the ultra performance liquid chromatography in the step (6) are as follows: a chromatographic column:
BEHC 181.7 μm 2.1mm X50 mm column; column temperature: 30 ℃, mobile phase a: acetonitrile, mobile phase B: water; isocratic elution procedure, flow phase ratioExamples are 60% a, 40% B, column flow: 0.2mL/min, sample size: 1 μ L, assay time: 5min, detection wavelength of formaldehyde: 365nm and an ultraviolet detector.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention prepares a series of low-concentration standard working solutions, so that the concentration of formaldehyde in the additive used by the company falls within the range of a standard working curve, thereby improving the accuracy of data.
(2) The detection time is short: the period of the invention for determining the formaldehyde in the additive for the cigarette only needs 5 minutes.
(3) The detection method provided by the invention is simple, convenient and accurate, and has good repeatability and high sensitivity.
(4) The detection method adopted by the invention greatly shortens the analysis time, reduces the loss of the mobile phase and reduces the pollution to the environment.
Drawings
FIG. 1 is a chromatogram of a standard working solution;
FIG. 2 is a chromatogram of a sample of the additive of example 1.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
(1) Preparation of standard working solutions: preparing a standard working solution containing formaldehyde-2, 4-dinitrophenylhydrazone with 6 levels and a certain concentration gradient, wherein the method comprises the following steps: accurately transferring 0.5mL of 1.0mg/mL of formaldehyde-2, 4-dinitrophenylhydrazone into a 50mL volumetric flask by using a pipette, and fixing the volume of acetonitrile to be determined as a grade 1 standard solution. And (3) adding 20.00mL of the grade 1 standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a grade 2 standard solution. And (3) adding 20.00mL of the grade 2 standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a grade 3 standard solution. And (3) taking 20.00mL of the grade 3 standard solution, adding the grade 3 standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a grade 4 standard solution. And (3) taking 20.00mL of the 4 th-grade standard solution, adding the solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 5 th-grade standard solution. And (3) adding 20.00mL of the 5 th-grade standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 6 th-grade standard solution.
(2) Preparation of derivatization reagent: 0.1g of 2, 4-dinitrophenylhydrazine is weighed into a 100mL brown volumetric flask, 0.5mL of phosphoric acid is added, and acetonitrile is used for constant volume to prepare a 2, 4-dinitrophenylhydrazine acetonitrile phosphoric acid solution (the concentration of the 2, 4-dinitrophenylhydrazine is 1.0 mg/mL).
(3) Preparation of extraction solution: preparation of tetrahydrofuran-water (THF-H)2O) solution, tetrahydrofuran: water (9:1) (volume ratio).
(4) Preparation of sample solution: weighing 1g of a sample of the tobacco additive (accurate to 0.1mg) and placing the sample in a 50mL conical flask with a plug, adding 20.00mL of extraction solution, fully and uniformly mixing, placing the sample in a rotary oscillator, rotationally oscillating the sample at 100rpm for 5min, standing the sample for 1min, accurately transferring 1mL of supernatant into a 10mL volumetric flask, accurately transferring 1mL of derivatization reagent, fixing the volume of the extraction solution, placing the solution for 10min for derivatization, and filtering the solution by using a 0.22 mu m organic filter membrane to obtain a filtrate, namely a sample solution.
(5) Blank test: and (5) repeating the step without adding the sample, and performing ultra performance liquid chromatography analysis.
(6) Ultra-high performance liquid chromatography analysis: and respectively detecting and analyzing the standard working solution, the sample solution and the blank test solution with 6 concentration levels by using an ultra-high performance liquid chromatograph. The specific analysis conditions were as follows: a chromatographic column:
BEHC 181.7 μm 2.1mm X50 mm column; column temperature: at 30 ℃. Mobile phase A: acetonitrile, mobile phase B: water; isocratic elution procedure, mobile phase ratio 60% a, 40% B, column flow: 0.2mL/min, sample size: 1 μ L, assay time: 5min, detection wavelength of formaldehyde: 365nm and an ultraviolet detector. The detection chromatogram is shown in FIG. 1.
(7) Establishing a standard working curve: converting formaldehyde-2, 4-dinitrophenylhydrazone into formaldehyde concentration, and establishing a working curve of the standard working solution by using a peak area which is equivalent to the area where the equivalent concentration of the formaldehyde corresponds to the formaldehyde-2, 4-dinitrophenylhydrazone in the standard working solution.
(8) And (4) calculating a result: substituting the chromatographic peak area of the formaldehyde-2, 4-dinitrophenylhydrazone of the sample solution measured under the same condition into the standard working curve obtained in the step (7) to obtain the concentration of the formaldehyde, thereby obtaining the content of the formaldehyde in the additive sample.
Determining a sample according to instrument test conditions, and quantitatively obtaining the content of formaldehyde in the liquid to be tested by using retention time qualitative and external standard method, wherein the formula is as follows:
in the formula: x represents the formaldehyde content in the sample in mg/kg;
c-formaldehyde concentration in mg/L from the standard curve;
C0-blank values, in mg/L, from the standard curve;
k is the dilution multiple;
v is volume of extract in mL;
m is the mass of the sample in g.
The formaldehyde content of the tobacco additive sample used in example 1 was calculated to be 5.7 mg/kg.
Example 2
Methodology investigation:
1. the standard curve and detection limit of the method of embodiment 1 of the invention are as follows: preparing 6-grade standard working solution containing formaldehyde-2, 4-dinitrophenylhydrazone with a certain concentration gradient; converting the formaldehyde-2, 4-dinitrophenylhydrazone into formaldehyde concentration, establishing a standard working curve by using a peak area which is equivalent to the equivalent concentration of the formaldehyde and corresponds to the formaldehyde-2, 4-dinitrophenylhydrazone in the standard working solution, and performing linear regression to obtain a regression equation and a correlation coefficient. The amounts at which the S/N-ratio is 10 and S/N-3, respectively, are used as the quantitation limit and the detection limit, and the results are shown in Table 1.
TABLE 1 regression equation, correlation coefficient, quantitation limit, and detection limit for Formaldehyde-2, 4-dinitrophenylhydrazone
2. And (3) precision test: preparing a sample solution to be detected according to the method in the embodiment 1, precisely absorbing the same sample solution to be detected, continuously injecting samples for 6 times in the same day according to the specified chromatographic conditions, recording the peak area of formaldehyde-2, 4-dinitrophenylhydrazone in the sample, and calculating the RSD value of the peak area. The results are shown in Table 2, and the RSD value of the peak area of the formaldehyde-2, 4-dinitrophenylhydrazone is 2.11%, which shows that the precision of the instrument is good. And (3) continuously taking 3 days, precisely absorbing the sample solution to be detected every day, continuously feeding samples for 3 times in the same day according to specified chromatographic conditions, recording the peak area of the formaldehyde-2, 4-dinitrophenylhydrazone for 3 days, and calculating the RSD value of the peak area. The results are shown in Table 2, and the RSD value of the peak area of the formaldehyde-2, 4-dinitrophenylhydrazone is 2.61%, which shows that the day precision of the instrument is good.
3. And (3) repeatability test: 6 parts of the same additive sample are precisely weighed, a sample solution to be detected is prepared according to the method in the embodiment 1, sample injection measurement is carried out according to specified chromatographic conditions, and the calculated peak area RSD value of formaldehyde-2, 4-dinitrophenylhydrazone in the sample is 1.50 percent as shown in the table 2, which indicates that the method has good repeatability.
TABLE 2 Formaldehyde-2, 4-dinitrophenylhydrazone precision, repeatability
4. And (3) standard recovery rate test: precisely weighing 9 parts of additive sample with the known content of 5.7mg/kg, and precisely adding three types of formaldehyde-2, 4-dinitrophenylhydrazone with different contents according to 50%, 100% and 150% of the formaldehyde content in the sample solution to be detected. The sample solution to be tested was prepared as described in example 1, and the sample injection measurement was performed under the prescribed chromatographic conditions, and the recovery rate of spiked sample and the relative standard deviation were calculated, and the results are shown in the table. As can be seen from Table 3, the average recovery rate of formaldehyde is 90.8% -103.1%, which indicates that the method is accurate and reliable and is suitable for analyzing formaldehyde in the additive sample.
TABLE 3 results of recovery measurements with addition of standard
All the above tests require blank test detection.
Claims (5)
1. A method for rapidly determining formaldehyde in a tobacco additive is characterized by comprising the following steps:
(1) preparation of standard working solutions: preparing 6-grade standard working solution with concentration gradient, which contains formaldehyde-2, 4-dinitrophenylhydrazone;
(2) preparation of derivatization reagent: weighing 2, 4-dinitrophenylhydrazine in a brown volumetric flask, adding phosphoric acid, and diluting to the constant volume with acetonitrile to prepare a 2, 4-dinitrophenylhydrazine acetonitrile phosphoric acid solution;
(3) preparation of extraction solution: preparing tetrahydrofuran-water solution;
(4) preparation of sample solution: weighing 1g, accurately measuring to 0.1mg, placing a sample in a 50mL conical flask with a plug, adding 20.00mL of extraction solution, fully and uniformly mixing, placing in a rotary oscillator, rotationally oscillating at 100rpm for 5min, standing for 1min, accurately transferring 1mL of supernatant into a 10mL volumetric flask, accurately transferring 1mL of derivatization reagent, fixing the volume of the extraction solution, placing for 10min for derivatization, filtering with a 0.22 mu m organic filter membrane, and obtaining a filtrate which is a sample solution;
(5) blank test: repeating the rest steps in the step (4) without adding a sample;
(6) ultra-high performance liquid chromatography analysis: respectively detecting and analyzing the standard working solution, the sample solution and the blank test solution with 6 concentration levels by using an ultra-high performance liquid chromatograph;
(7) establishing a standard working curve: converting formaldehyde-2, 4-dinitrophenylhydrazone into formaldehyde concentration, and establishing a working curve of the standard working solution by using a peak area which is equivalent to the area where the equivalent concentration of the formaldehyde corresponds to the formaldehyde-2, 4-dinitrophenylhydrazone in the standard working solution;
(8) and (4) calculating a result: substituting the chromatographic peak area of the formaldehyde-2, 4-dinitrophenylhydrazone of the sample solution measured under the same condition into the standard working curve obtained in the step (7) to obtain the concentration of the formaldehyde, thereby obtaining the content of the formaldehyde in the additive sample.
2. The method for rapidly determining formaldehyde in the cigarette additive according to claim 1, wherein the specific preparation method of the standard working solution in the step (1) is to accurately transfer 0.5mL1.0mg/mL formaldehyde-2, 4-dinitrophenylhydrazone into a 50mL volumetric flask by using a pipette, and fix the volume of acetonitrile to be the 1 st-level standard solution; adding 20.00mL of the 1 st-grade standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 2 nd-grade standard solution; adding 20.00mL of the grade 2 standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a grade 3 standard solution; adding 20.00mL of the 3 rd-level standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to be determined as a 4 th-level standard solution; adding 20.00mL of the 4 th-level standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 5 th-level standard solution; and (3) adding 20.00mL of the 5 th-grade standard solution into a 50mL volumetric flask, and fixing the volume of acetonitrile to obtain a 6 th-grade standard solution.
3. The method for rapidly determining formaldehyde in the cigarette additive according to claim 1, wherein the derivatization reagent in the step (2) is prepared by weighing 0.1g of 2, 4-dinitrophenylhydrazine in a 100mL brown volumetric flask, adding 0.5mL of phosphoric acid, and diluting to constant volume with acetonitrile to prepare a 2, 4-dinitrophenylhydrazine acetonitrile phosphoric acid solution with a 2, 4-dinitrophenylhydrazine concentration of 1.0 mg/mL.
4. The method for rapidly determining formaldehyde in the tobacco additive according to claim 1, wherein in the step (3), tetrahydrofuran: the volume ratio of water was 9: 1.
5. The method for rapidly determining formaldehyde in the tobacco additive according to claim 1, wherein specific conditions of the ultra-high performance liquid chromatography in the step (6) are as follows: a chromatographic column: ACQUITYUPLC columns of BEHC 181.7 μm 2.1mm X50 mm; column temperature: 30 ℃, mobile phase a: acetonitrile, mobile phase B: water; isocratic elution procedure, mobile phase ratio 60% a, 40% B, column flow: 0.2mL/min, sample size: 1 μ L, assay time: 5min, detection wavelength of formaldehyde: 365nm and an ultraviolet detector.
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| CN115248257A (en) * | 2021-04-26 | 2022-10-28 | 湖南中烟工业有限责任公司 | Preparation and detection method of sample to be detected of formaldehyde in packaging material |
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Application publication date: 20201030 |