CN111157645B - High performance liquid chromatography-tandem mass spectrometry method for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction - Google Patents
High performance liquid chromatography-tandem mass spectrometry method for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction Download PDFInfo
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Abstract
The invention provides a high performance liquid chromatography tandem mass spectrometry method for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction, which integrates purification and extraction, firstly, a proper amount of extractant is added into a sample, an ultrasonic-assisted technology is combined, a target object in the sample is rapidly extracted, then, the sample is centrifuged, layered and extracted to obtain a part of clear liquid, a PSA purifying agent is added, the purification process is accelerated by vortex assistance, and then, supernatant obtained by centrifugation passes through an organic membrane and then enters a high performance liquid chromatography tandem mass spectrometer for analysis; the invention applies the dispersed solid phase extraction technology, simplifies the pretreatment process, saves the treatment time, can be suitable for the pretreatment of most food contact packaging paper in the market, has the advantage of batch operation, can detect 6 quaternary ammonium salts with different structural types at one time, and is simple, convenient and efficient.
Description
Technical Field
The invention relates to an analysis method of quaternary ammonium salt in food packaging paper, and particularly relates to a high performance liquid chromatography tandem mass spectrometry method for determining quaternary ammonium salt bacteriostatic agent in food bacteriostatic packaging paper based on a dispersive solid-phase extraction technology.
Background
Food safety issues have been a major concern for livelihood in recent years, and much attention has been focused on substances harmful to the human body, which are directly added to foods, but packaging materials which are actually in direct contact with foods are also closely related to our food safety issues. A large number of food packaging materials made of different materials exist in the market at present, and manufacturers often add different chemical additives to achieve certain special properties of the materials in the production process of the manufacturers. The paper packaging material has the characteristics of good performance, reproducibility and the like, is an important packaging material in food packaging industry at home and abroad, and the use safety problem of the paper packaging material also needs to draw attention.
Bacteriostatic agents are chemical agents that can effectively control or kill microorganisms in a system, and can be classified into active chlorides, inorganic compounds, organic acid salts, quaternary ammonium salts, phenols, organic sulfur compounds, organic metals, and others according to their properties or structures. The quaternary ammonium salt bactericide has good applicability and high bactericidal capacity, and is widely used. In the production of paper packaging paper, manufacturers add reagents with antibacterial properties to sample paper by using relevant processes such as spraying, sizing, coating and dipping to achieve the purpose of better storing perishable food, so that the paper has certain antibacterial performance, and then the antibacterial paper packaging material is prepared. In addition, preservatives of quaternary ammonium salts can be used in the wood preservation process, and the quaternary ammonium salts can enter the food packaging paper, so that the potential risk of food pollution is caused. Researches show that quaternary ammonium has strong toxicity to aquatic organisms and can cause diseases such as asthma, skin anaphylactic reaction, hypopsia and the like of human beings, and the upper limit of the residual quaternary ammonium salt in food is regulated to be 0.1mg/kg by European food safety administration. In view of the above situation, establishing a rapid and effective detection method has great significance for accurate detection and risk assessment of quaternary ammonium salt in food packaging materials.
At present, the detection method of the quaternary ammonium salt bacteriostatic agent mainly relates to an ultraviolet-visible spectrophotometry method, a capillary electrophoresis method, a liquid chromatography-mass spectrometry/mass spectrometry method and the like, mainly belongs to the field of research of environmental water samples, soil, sediments and the like, and has less research on food packaging materials. In modern analysis work, sample pretreatment plays a crucial role, especially for complex matrixes, the scientific pretreatment method can not only reduce the matrix effect and improve the enrichment multiple, but also can even greatly simplify the analysis process and directly influence the advantages and disadvantages of the analysis method. The dispersive solid-phase extraction is simple and convenient to operate, can effectively remove interference factors, and is a very effective pretreatment technology. The mass spectrum has high selectivity, high analysis speed and high sensitivity, and the quaternary ammonium salt can be more accurately and quickly analyzed after the high performance liquid chromatography is combined. Therefore, the invention provides a method for detecting quaternary ammonium salt bacteriostatic agents in food packaging paper by combining the current effective pretreatment technology and the forward-edge mass spectrometry technology, integrates extraction and purification, can detect 6 quaternary ammonium salts with different structure types at one time, and has the characteristics of simplicity, convenience and high efficiency.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to establish a high performance liquid chromatography tandem mass spectrometry method for determining quaternary ammonium salt bacteriostat in food bacteriostasis packaging paper based on a dispersive solid-phase extraction technology.
The method integrates purification and extraction, firstly, a proper amount of extractant is added into a sample, and an ultrasonic auxiliary technology is combined to rapidly extract a target object in the sample. And then centrifuging the sample, layering and extracting a part of clear liquid, adding a PSA purifying agent, accelerating the purification process by vortex assistance, centrifuging to obtain supernatant, passing the supernatant through an organic membrane, and entering a high performance liquid chromatography tandem mass spectrometer for analysis.
The pretreatment method has the advantages of simple required equipment, simple and convenient operation and short operation time, can be suitable for pretreatment of most food contact packaging paper in the market, and has the advantage of batch operation. The quaternary ammonium salt in the food packaging paper measured by the invention is at least one of the following compounds: tetramethylammonium chloride, dodecyldimethylbenzylammonium bromide, dodecyltrimethylammonium chloride, tetradecyldimethylbenzylammonium chloride, hexadecyldimethylbenzylammonium chloride, and didecyldimethylammonium chloride.
The technical scheme of the invention is as follows:
a high performance liquid chromatography tandem mass spectrometry method for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction comprises the following steps:
(1) Sample pretreatment
Crushing dried food packaging paper, adding methanol, performing ultrasonic extraction (3 min), centrifuging (12000rpm, 5 min), mixing an upper organic layer with a purifying agent PSA (N-propylethylenediamine), performing vortex (2 min), centrifuging (8000rpm, 3 min), and allowing a supernatant to pass through an organic membrane (with the aperture of 0.2 mu m) to obtain a sample solution to be detected;
the ratio of the pulverized food packaging paper sample (in g) to methanol (in mL) was 1:10;
the ratio of scavenger PSA (in g) to the organic layer taken (in mL) was 0.1:1;
(2) Sample detection
Injecting the sample solution to be detected obtained in the step (1) into a high performance liquid chromatography tandem mass spectrometry system for analysis, wherein the method adopts a partial sample introduction, gradient elution and multi-reaction monitoring mode, obtains parent ions through first-stage mass spectrometry scanning, selects 2 groups of target characteristic ion pairs through second-stage mass spectrometry scanning for qualitative and quantitative determination, and finally obtains a sample total ion flow graph and a selected ion flow graph;
high performance liquid chromatography conditions: column C18 (2.1 mm. Times.50mm, 1.7 μm); gradient leaching: a-5mmol/L ammonium acetate water solution, B-5mmol/L ammonium acetate methanol solution; 0.00-0.50min, 30% by weight of A; 0.50-2.00min, 30-10% of A; 2.00-4.00min, 10-2% A; 4.00-6.50min, 2-0% of A;6.50 to 6.60min,0 to 30 percent of A; 6.60-7.00min, 30% A;
mass spectrum conditions: assembling ESI ionization source by Perkin Elmer Qsight series triple quadrupole mass spectrometry, and adopting a positive source mode; the ionization voltage is 4000V; the ion source temperature is 350 ℃; back blowing dry gas at 100 μ L/min; atomizing gas 180 mu L/min; all the used gases are high-purity nitrogen; entrance voltage, collision energy, characteristic ion pairing are shown in Table 1 () " a "is a quantitative ion pair);
the quaternary ammonium salt parent ion and the qualitative and quantitative ion pair (parent ion/qualitative ion/quantitative ion a) are as follows: tetramethylammonium chloride 74/42.1/58.1 a (ii) a Dodecyl dimethyl benzyl ammonium bromide 304/91.1/212.5 a (ii) a Dodecyl trimethyl ammonium chloride 228/57.1/60.2 a (ii) a Tetradecyl dimethyl benzyl ammonium chloride 332.4/240.5/91.1 a (ii) a Hexadecyl dimethyl benzyl ammonium chloride 360.5/268.5/91.1 a (ii) a Double tenAlkyl dimethyl ammonium chloride 326.5/57.2/186.4 a ；
(3) Establishing a standard curve
Taking a standard substance of tetramethylammonium chloride, dodecyl dimethyl benzyl ammonium bromide, dodecyl trimethyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, hexadecyl dimethyl benzyl ammonium chloride and didecyl dimethyl ammonium chloride, preparing a mixed standard stock solution by taking methanol-water (volume ratio is 1;
the concentration ranges of each standard in the paper sample are as follows:
0.1-50 mu g/kg of tetramethylammonium chloride; dodecyl dimethyl benzyl ammonium bromide 0.1-100 microgram/kg; dodecyl trimethyl ammonium chloride 0.1-50 microgram/kg; tetradecyl dimethyl benzyl ammonium chloride 0.1-50 μ g/kg; 0.1-100 mug/kg of hexadecyl dimethyl benzyl ammonium chloride; 0.1-50 mug/kg of didecyl dimethyl ammonium chloride;
the characteristic peaks of each standard substance in a total ion flow diagram of a high performance liquid chromatography tandem mass spectrum are as follows:
tetramethylammonium chloride for 0.74min; dodecyl dimethyl benzyl ammonium bromide for 2.71min; dodecyl trimethyl ammonium chloride for 2.42min; tetradecyl dimethyl benzyl ammonium chloride for 3.19min; cetyl dimethyl benzyl ammonium chloride for 3.74min; didecyl dimethyl ammonium chloride for 3.30min;
(4) Obtaining qualitative and quantitative results of quaternary ammonium salt in sample
Qualitative determination is carried out on quaternary ammonium salt contained in the sample through comparison of the target substance qualitative ion pair and the standard substance qualitative ion pair in the sample to be detected;
substituting the quantitative ion pair characteristic peak area value of the target object in the sample HPLC-MS selected ion flow diagram obtained in the step (2) into the standard curve obtained in the step (3), and calculating to obtain the content of the quaternary ammonium salt in the sample.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides an effective method for extracting quaternary ammonium salt bacteriostatic agents from paper for food packaging.
2. The invention uses the dispersed solid phase extraction technology, simplifies the pretreatment process and saves the treatment time.
Drawings
FIG. 1 is a chemical structural diagram of each quaternary ammonium salt in example 1;
FIG. 2 shows the results of the optimization of the type of extractant used in example 1;
FIG. 3 shows the results of the optimization of the volume of the extractant in example 1;
FIG. 4 shows the optimization results of the extraction time in example 1;
FIG. 5 shows the results of optimizing the type of the scavenger in example 1;
FIG. 6 shows the results of optimizing the amount of the scavenger used in example 1;
FIG. 7 is an ion flow diagram of the extraction of quaternary ammonium salts in the standard-added food packaging paper in example 1, wherein the standard-added concentration of each substance is 10 mug/kg.
Detailed Description
The invention is further described below by means of specific examples, without the scope of protection of the invention being limited thereto.
The chemical information of the quaternary ammonium salt related to the invention is shown as follows:
example 1: detection of quaternary ammonium salt in food antibacterial packaging paper
(1) Sample pretreatment
Cutting dried food packaging paper into fragments smaller than 0.5cm multiplied by 0.5cm, accurately weighing 1.0g of bacteriostatic paper sample in a 50mL conical flask, adding 10mL of methanol by using a liquid transfer gun, performing ultrasonic extraction for 3min, then centrifuging at 12000r/min for 5min, accurately extracting 1mL of an organic layer, transferring the organic layer to a centrifuge tube filled with 100mg of PSA purifying agent in advance, performing vortex for 2min, then centrifuging at 8000r/min for 3min, and extracting a supernatant to pass through an organic film to wait for detection by an instrument.
(2) Sample detection
High performance liquid chromatography conditions: column C18 column (2.1 mm. Times.50mm, 1.7 μm). Gradient elution: a-5mmol/L ammonium acetate water solution and B-5mmol/L methanol solution; 0.00 to 0.50min,30% by weight A; 0.50-2.00min, 30-10% of A; 2.00-4.00min, 10-2% A; 4.00-6.50min, 2-0% A; 6.50-6.60min, 0-30% A;6.60 to 7.00min,30% by weight.
The mass spectrum conditions are as follows: assembling ESI ionization source by PerkinElmer Qsight series triple quadrupole mass spectrometry, and adopting a positive source mode; the ionization voltage is 4000V; the ion source temperature is 350 ℃; back blowing dry gas at 100 μ L/min; atomizing gas 180 mu L/min; entrance voltage, collision energy, characteristic ion pairing are shown in Table 1 () " a "is a quantitative ion pair); the gas used is high purity nitrogen.
TABLE 1 Quaternary ammonium salt Inlet Voltage, collision energy, characteristic ion pairs
(3) Establishing a standard curve
Taking a standard substance of tetramethylammonium chloride, dodecyldimethylbenzyl ammonium bromide, dodecyltrimethylammonium chloride, tetradecyldimethylbenzyl ammonium chloride, hexadecyldimethylbenzyl ammonium chloride and didecyldimethylammonium chloride, preparing a mixed standard stock solution by using methanol-water (volume ratio is 1.
TABLE 2 Linear equation, linear Range, linear correlation coefficient, detection limit, quantitative limit, etc. indexes of quaternary ammonium salt
(4) Method evaluation
The recovery rate of the standard addition of the method, the daily precision and the daily precision are examined under the conditions of the method to evaluate the accuracy and the reproducibility of the method, and the results show that the recovery rate of each target object is 79-113%, the daily precision is less than 8.9% and the daily precision is less than 8.8%, and the method shows good accuracy and reproducibility, and the specific results are shown in table 3.
TABLE 3 Quaternary ammonium salt methodological index
Claims (5)
1. A high performance liquid chromatography tandem mass spectrometry method for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction is characterized by comprising the following steps:
(1) Sample pretreatment
Crushing dried food packaging paper, adding methanol, performing ultrasonic extraction, centrifuging, mixing an upper organic layer with a purifying agent PSA, performing vortex and centrifugation, and passing a supernatant through an organic membrane to obtain a sample solution to be detected;
(2) Sample detection
Injecting the sample solution to be detected obtained in the step (1) into a high performance liquid chromatography tandem mass spectrometry system for analysis, wherein the method adopts a partial sample introduction, gradient elution and multi-reaction monitoring mode, obtains parent ions through first-stage mass spectrometry scanning, selects 2 groups of target characteristic ion pairs through second-stage mass spectrometry scanning for qualitative and quantitative determination, and finally obtains a sample total ion flow graph and a selected ion flow graph;
high performance liquid chromatography conditions: a chromatography column C18 column; gradient elution: a-5mmol/L ammonium acetate water solution, B-5mmol/L ammonium acetate methanol solution; 0.00 to 0.50min,30 percent of A;0.50 to 2.00min,30 to 10 percent A;2.00 to 4.00min,10 to 2 percent A;4.00 to 6.50min,2 to 0% A;6.50 to 6.60min,0 to 30% A; 30% of A in 6.60-7.00 min;
mass spectrum conditions: assembling ESI ionization source by Perkin Elmer Qsight series triple quadrupole mass spectrometry, and adopting a positive source mode; the ionization voltage is 4000V; the ion source temperature is 350 ℃; back blowing dry gas at 100 μ L/min; atomizing gas 180 mu L/min; all the used gases are high-purity nitrogen; inlet voltage, collision energy, characteristic ion pairs are shown in the following Table, wherein " a "is a quantitative ion pair:
(3) Establishing a standard curve
Taking standard substances of tetramethylammonium chloride, dodecyl dimethyl benzyl ammonium bromide, dodecyl trimethyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, hexadecyl dimethyl benzyl ammonium chloride and didecyl dimethyl ammonium chloride, preparing a mixed standard stock solution by taking methanol-water as a solvent, diluting the obtained mixed standard stock solution to a series of concentrations, respectively coating the concentrations on paper for packaging negative food, after fully adsorbing for 24 hours, pretreating the obtained labeled paper sample according to the pretreatment method in the step (1), analyzing the pretreated paper sample under the detection method in the step (2), obtaining a high performance liquid chromatography-tandem mass spectrometry extraction ion flow diagram of the standard substances, and drawing a standard curve by taking the area of a quantitative ion pair peak in the extraction ion flow diagram as a vertical coordinate and the concentration of each quaternary ammonium salt in the paper sample as a horizontal coordinate;
(4) Obtaining qualitative and quantitative results of quaternary ammonium salt in sample
Qualitative determination is carried out on quaternary ammonium salt contained in the sample through the comparison of the target object qualitative ion pair and the standard substance qualitative ion pair in the sample to be detected;
substituting the quantitative ion pair characteristic peak area value of the target object in the sample HPLC-MS selected ion flow diagram obtained in the step (2) into the standard curve obtained in the step (3), and calculating to obtain the content of the quaternary ammonium salt in the sample.
2. The high performance liquid chromatography-tandem mass spectrometry for measuring quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction as claimed in claim 1, wherein in the step (1), the mass-to-volume ratio of the crushed paper for food packaging to methanol is 1:10,g/mL.
3. The high performance liquid chromatography-tandem mass spectrometry for measuring quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction as claimed in claim 1, wherein in the step (1), the mass-to-volume ratio of the scavenger PSA to the taken organic layer is 0.1:1,g/mL.
4. The HPLC tandem mass spectrometry for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction as claimed in claim 1, wherein in step (3), the concentration range of each standard substance in the paper sample is as follows:
0.1 to 50 mu g/kg of tetramethylammonium chloride; 0.1 to 100 mu g/kg of dodecyl dimethyl benzyl ammonium bromide; 0.1 to 50 mu g/kg of dodecyl trimethyl ammonium chloride; tetradecyl dimethyl benzyl ammonium chloride is 0.1 to 50 mu g/kg; 0.1 to 100 mu g/kg of hexadecyl dimethyl benzyl ammonium chloride; 0.1 to 50 mu g/kg of didecyl dimethyl ammonium chloride.
5. The high performance liquid chromatography-tandem mass spectrometry for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction as claimed in claim 1, wherein in the step (3), characteristic peaks of each standard substance in a total ion flow chart of the high performance liquid chromatography-tandem mass spectrometry are as follows:
tetramethylammonium chloride for 0.74min; dodecyl dimethyl benzyl ammonium bromide for 2.71min; dodecyl trimethyl ammonium chloride for 2.42min; tetradecyl dimethyl benzyl ammonium chloride for 3.19min; hexadecyl dimethyl benzyl ammonium chloride for 3.74min; didecyl dimethyl ammonium chloride for 3.30 min.
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