CN113702516B - Detection method of antibacterial and mildew-proof agent in bamboo and wood products - Google Patents
Detection method of antibacterial and mildew-proof agent in bamboo and wood products Download PDFInfo
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Abstract
The invention relates to the technical field of detection, in particular to a detection method of an antibacterial mildew preventive in bamboo products. The invention adopts two extraction methods of QuEhERS method and solid phase extraction, and uses BEHC 18 Separating by chromatographic column, gradient eluting with acetonitrile-10 mmol/L ammonium acetate solution as mobile phase, electrospraying positive and negative ions by tandem mass spectrometry, detecting by multi-reaction monitoring (MRM) mode, and quantifying by external standard method. And (3) determining the content of the mildew-proof and antibacterial agents in the bamboos and the woods by adopting ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS). The detection method provided by the invention can be used for rapidly and accurately detecting 16 antibacterial and mildew-proof agents in bamboo products, so that effective monitoring of bamboo food related products is enhanced.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a detection method of an antibacterial mildew preventive in bamboo products.
Background
The related products of the bamboo food are mainly processed by a physical processing mode in the past, but the bamboo food contains rich nutrient substances, mainly comprises lignin, cellulose, hemicellulose, pectin, starch, protein, fat and the like, namely the development of biological pretreatment research on anaerobic digestion of cellulose biomass is easy to mildew in a humid environment; in addition, the bamboo material also contains insect pests, ova and the like, so that insect leeches are easy to generate in the material, mould can be quickly spread due to the existence of insect pests, and the water activity in the local material is improved, so that the mould rot of the bamboo material is aggravated.
In order to improve the utilization of bamboo and wood, according to the characteristics of easy corrosion and mildew of the bamboo and wood, besides the physical and mechanical processing of the bamboo and wood, the corrosion prevention, mildew prevention and insect prevention treatment is also carried out by a three-proofing chemical method so as to prevent the phenomena of decay, mildew and insect and leech, but in contrast, the application of the three-proofing chemical processing method also introduces corresponding risk substances, such as chemical preservatives including sulfur-containing boiling agents, thiabendazole, o-phenylphenol, biphenyl, imazalil and the like, and enterprises have no strict control measures due to weak technical strength and poor safety control, so that the risk of exceeding the standard of residues of the chemical preservatives in products is increased, thereby leading to the potential safety hazard of the bamboo and wood products for foods. In addition, some bamboo and wood raw materials are extremely easy to mildew and rot, and are usually required to be subjected to corrosion prevention treatment in time after being cut down, and because some bamboo and wood raw materials are not specially used for producing food related products, the bamboo and wood raw materials are generally treated according to industrial bamboo and wood materials in the three-proofing treatment, so that certain preservative chemicals such as pentachlorophenol and the like which are commonly used in the industrial bamboo and wood materials and are forbidden in the food bamboo and wood materials can be used.
The antibacterial and antimycotic agent of bamboo and wood has corresponding detection methods only in the national standard regulation such as thiabendazole, o-phenylphenol, biphenyl, imazalil, pentachlorophenol and the like. The effective component of the bamboo anti-II commonly used in actual production takes the bactericide MBT as a main body and is matched with a certain amount of pesticide SFS and the like to form a composite preparation. In addition, in the field investigation of related products of bamboo and wood foods, manufacturers use bamboo to prevent II, entomomycetin and sulfur dioxide fumigation, even if common household unknown insect prevention and mildew preventive agents such as methyl 3-iodo-2-propyl butylcarbamate, didecyl dimethyl ammonium chloride, 2, 5-dichloro-3-bromophenol, sodium pentachlorophenate, chlorothalonil, carbendazim, imazalil, thiabendazole, aldicarb, tebuconazole, dimethyl fumarate, lindane, benzothiadiazole, sodium benzoate, potassium sorbate, 8-hydroxyquinoline copper, natamycin, captan, sulfur dioxide, salicylanilide, o-phenylphenol, thiabendazole, methyl parahydroxybenzoate, propyl parahydroxybenzoate, butyl parahydroxybenzoate, formaldehyde, glutaraldehyde, benzyl alcohol, biphenyl and the like are not established at present, so related products of bamboo and wood foods cannot be effectively monitored, and thus, great potential safety hazards exist.
Disclosure of Invention
Aiming at the problem that the existing bamboo-wood related products cannot be effectively monitored due to incomplete detection means, the invention provides a detection method of an antibacterial mildew preventive in bamboo-wood products, which can simultaneously detect a plurality of antibacterial mildew preventive in bamboo-wood food related products and effectively reduce potential safety hazards of the bamboo-wood products.
The detection method of the antibacterial mildew preventive in the bamboo products is characterized by comprising the following steps of:
s1, sample pretreatment: sample treatment is carried out by adopting a QuEhERS method or a solid-phase extraction method;
the QuEhERS method is adopted: weighing 1g of sample, adding 5mL of water into a 50mL plastic centrifuge tube, accurately adding 10.0mL of methanol, covering a cover, shaking uniformly, performing ultrasonic extraction for 30 minutes, adding a QuEChERS Extract Tubes EN Method extraction reagent pack, performing vortex extraction for 2min, performing centrifugation for 3 minutes at 5000 rpm, sucking 4mL of supernatant, placing the supernatant into a QuEChERS purification reagent tube, performing vortex 30s, performing centrifugation for 3 minutes at 3000 rpm, taking 1.0mL of the supernatant into a nitrogen blowing tube, performing nitrogen blow-drying at 45 ℃, accurately adding 1.0mL of acetic acid-methanol mixed solution for dissolution, filtering with a 0.45 mu m organic phase filter membrane, and performing test;
the solid phase extraction method comprises the following steps: weighing 1g of sample, adding 10mL of methanol-water solution containing 0.1% formic acid into a 50mL plastic centrifuge tube, covering a cover, shaking uniformly, performing ultrasonic extraction for 30 minutes, centrifuging at 5000 rpm for 3 minutes, taking 1.0mL of clear liquid, adding 1mL of water into the centrifuge tube, diluting, purifying by using an oasis MCX solid phase extraction column, controlling the column passing speed to be 1 drop/second, washing the extraction column by using 3mL of water and 3mL of methanol after the sample liquid passes through the column, performing vacuum pumping, eluting by using 10mL of 5% ammonia water-methanol solution, collecting eluent, drying by nitrogen at 45 ℃, accurately adding 1.0mL of acetic acid-methanol mixed solution for dissolution, filtering by using a 0.45 mu m organic phase filter membrane, and testing;
s2, sample detection: the sample extracting solution is detected by adopting ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry, and the detection conditions are as follows:
LC-MS/MS liquid phase conditions: comprises a chromatographic column: ACQUITY UPLC BEH C18; the mobile phase A is acetonitrile, the mobile phase B is acetic acid, and the mobile phase A contains 0.1% formic acid aqueous solution, and the column temperature is as follows: room temperature;
LC-MS/MS mass spectrometry conditions: ionization mode: ESI (electronic service provider interface) + And ESI (electronic service interface) - The method comprises the steps of carrying out a first treatment on the surface of the Capillary voltage: 2.83kV; ion source temperature: 150 ℃; desolventizing gas temperature: 500 ℃; desolventizing gas flow: 800L/hr; scanning mode: MRM mode; collision gas: helium gas;
s3, analyzing results: in ionization mode ESI + And ESI (electronic service interface) - And (3) performing full scanning on the standard solution in a mode to obtain molecular ions of a standard substance, performing secondary mass spectrometry on the molecular ions, selecting two characteristic fragment ions with larger signal intensity and stable signal, selecting the quantitative ion with the strongest relative abundance and the qualitative ion with the weaker relative abundance, drawing a standard curve, and quantifying the sample by an external standard method.
Further, after the nitrogen in the step S1 is dried, the acetic acid-methanol mixed solution is added, wherein the volume ratio of the acetic acid to the methanol is 8:2.
Further, in the methanol-water solution containing 0.1% formic acid added in the solid phase extraction method, the volume ratio of the methanol containing 0.1% formic acid to water is 1:1.
Further, the gradient elution conditions of the mobile phase in the LC-MS/MS liquid phase conditions are:
wherein, the mobile phase A and the mobile phase B are mixed according to volume percentage.
Preferably, the gradient elution condition of the mobile phase is as follows:
optimally, the gradient elution conditions of the mobile phase are as follows:
further, the sample injection amount in the step S2 is 5 μl.
Further, the antibacterial mildew preventive comprises any one or more of benzoic acid, dimethyl fumarate, methyl parahydroxybenzoate, ethyl parahydroxybenzoate, propyl parahydroxybenzoate, butyl parahydroxybenzoate, salicylanilide, o-phenylphenol, carbendazim, thiabendazole, 3-iodo-2-propyl butyl methyl carbamate, tebuconazole, didecyl dimethyl ammonium chloride, imazalil, pentachlorophenol and natamycin.
Further, specific mass spectrum conditions of the antibacterial mildew preventive are as follows:
wherein is the quantitative ion.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the detection method provided by the invention, the QuEhERS method and the solid-phase extraction method are adopted in the pretreatment stage, the target product can be extracted by the two extraction methods in the aspect of selectivity, the solid-phase extraction technology is slightly superior to the QUECHERS technology in the aspect of interference, the total scanning impurity peaks are relatively less, the mass spectrum target is clear and specific, and compared with the existing extraction mode, the recovery rate of the antibacterial mildew preventive is greatly improved.
(2) In the detection method provided by the invention, in the detection process, BEHC18 chromatographic column is used for separation, acetonitrile-10 mmol/L ammonium acetate solution is used as a mobile phase for gradient elution, the chromatographic peak-to-peak type obtained by separation is good, positive and negative ions are simultaneously scanned by tandem mass spectrometry electrospray with good separation degree, multi-reaction monitoring (MRM) mode detection is carried out, and the external standard method is used for quantification. The content of the mildew-proof and antibacterial agent in bamboo and wood is determined by adopting ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS), so that a more reliable basis is provided for the qualitative nature of the mildew-proof and antibacterial agent. The method is simple and convenient, is easy to operate, and can meet the requirements of rapid detection and confirmation.
In conclusion, the detection method provided by the invention can be used for effectively, rapidly and accurately detecting 16 common antibacterial and mildew-proof agents and pesticide insect-proof agents including benzoic acid, dimethyl fumarate, methyl parahydroxybenzoate, ethyl parahydroxybenzoate, propyl parahydroxybenzoate, butyl parahydroxybenzoate, salicylanilide, o-phenylphenol, carbendazim, thiabendazole, 3-iodo-2-propyl methyl butylcarbamate, tebuconazole, didecyl dimethyl ammonium chloride, imazalil, pentachlorophenol and natamycin in bamboo and wood food related products.
Description of the drawings:
FIG. 1 is a total ion flow chromatogram of a mixed standard solution of 16 mildewproof and antibacterial agents;
FIG. 2 is an ion diagram of benzoic acid obtained under optimal conditions;
FIG. 3 is an ion diagram of dimethyl fumarate obtained under optimal conditions;
FIG. 4 is an ion diagram of methyl parahydroxybenzoate obtained under optimal conditions;
FIG. 5 is an ion diagram of ethyl parahydroxybenzoate obtained under optimal conditions;
FIG. 6 is an ion diagram of propyl parahydroxybenzoate obtained under optimal conditions;
FIG. 7 is an ion diagram of butyl parahydroxybenzoate obtained under optimal conditions;
FIG. 8 is an ion diagram of salicylanilide obtained under optimal conditions;
FIG. 9 is an ion diagram of the ortho-phenylphenol obtained under optimal conditions;
FIG. 10 is an ion diagram of the production of carbendazim under optimal conditions;
FIG. 11 is an ion diagram of thiabendazole obtained under optimal conditions;
FIG. 12 is an ion diagram of the 3-iodo-2-propyl butyl methyl carbamate obtained under optimal conditions;
FIG. 13 is an ion diagram of tebuconazole obtained under optimal conditions;
FIG. 14 is an ion diagram of natamycin obtained under optimal conditions;
FIG. 15 is an ion diagram of imazalil obtained under optimal conditions;
FIG. 16 is an ion diagram of pentachlorophenol obtained under optimal conditions;
FIG. 17 is an ion diagram of pentachlorophenol obtained under optimal conditions;
Detailed Description
The invention is further illustrated below in connection with specific examples. It should be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. It is also to be understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the invention, and equivalents thereof fall within the scope of the invention as defined herein.
Details regarding the present invention are described below:
1. reagents and materials
Acetonitrile, methanol (chromatographic purity, fisher, usa); formic acid (superior purity, CNW company, germany); acetonitrile, methanol (analytically pure, tianjin, yongda chemical Co., ltd.); the experimental water is second-level ultrapure water (Milibo China Co., ltd.); nitrogen (purity greater than 99.99%, east cis gas limited in the forward region of bergamot); ammonium acetate (chromatographic purity, TEDIA company, germany)
16 antibacterial preservative standards: benzoic acid, dimethyl fumarate, methyl parahydroxybenzoate, ethyl parahydroxybenzoate, propyl parahydroxybenzoate, butyl parahydroxybenzoate, salicylanilide, o-phenylphenol, carbendazim, thiabendazole, methyl 3-iodo-2-propylbutylcarbamate, tebuconazole, didecyl dimethyl ammonium chloride, imazalil, pentachlorophenol, natamycin standard (purity not less than 98% in China national institute of metering).
2. Apparatus and device
ACQUITYTM ultra high performance liquid chromatography and WatersXevoTMTQMS triple quadrupole tandem mass spectrometer (Waters, USA); JP-C300 ultrasonic cleaner (Jeep ultrasonic electronic devices Co., ltd., guangzhou); 3-3KS high speed cryocentrifuge (Sigma Co., USA); DT-502A electronic balance (mature sheep weight instruments Co., ltd.); IKAMS3 vortex mixer (IKA company, germany); milli-Q deionized water generator (Millipore company, USA). ProElutMelamine solid phase extraction column (60 mg/3mL, di-Ma technologies Co., ltd.).
Example 1
Selection of chromatographic conditions
The invention examines the Shim-pack ODS-II (2.0 mm. D. Times.75 mm,1.6 μm), agilentSB-C 18 (2.1 mm. D.times.100 mm,1.8 μm) and ACQUITY
BEH C 18 (2.1 mm. D. Times.100 mm, 1.7. Mu.mm) separation effect of 3 types of columns on 5 types of mildewproof agents.
The results were as follows: ODS-II column thiabendazole and carbendazim are not completely separated, and a tailing phenomenon exists in chromatographic peaks; agilentSB-C 18 There are cases where the pentachlorophenol chromatographic peak is severely passivated;
BEHC 18 the chromatographic peak type obtained by chromatographic column separation is good, and the separation degree is good.
Example 2
Determination of sample pretreatment conditions
The bamboo and wood products have various components, complex matrix, and contain a large amount of compounds such as vitamins, flavone, organic acid and the like, and the matrix is severely interfered. The QUECHERS method is simple, convenient and quick, the organic solvent consumption of the solid phase extraction technology is small, the enrichment multiple is high, salicylanilide, o-phenylphenol, carbendazim, thiabendazole and tebuconazole are selected in the experiment, and the two methods of the solid phase extraction technology and the QUECHERS are adopted for extracting the related products of the bamboo and wood products, and the three aspects of selectivity, interference and recovery rate are compared.
The average recovery and relative standard deviation (n=6) for both extraction methods are as follows:
the experimental results show that: the two extraction methods can extract target products in the aspect of selectivity, the solid phase extraction technology is slightly superior to the QUECHERS technology in the aspect of interference, the total scanning impurity peaks are relatively less, but the mass spectrum target is clear and has strong specificity. The QUECHERS technology is higher than that of solid phase extraction
Example 3
The commercial bamboo chopsticks are used as samples for treatment and detection, and the method is as follows:
s1, sample pretreatment:
1g of the sample (accurate to 0.01 g) is weighed into a 50mL plastic centrifuge tube, 5mL of water is added, 10.0mL of methanol is accurately added, a cover is covered, shaking is carried out, ultrasonic extraction is carried out for 30 minutes, a QuEChERS Extract Tubes EN Method extraction reagent pack (Part No: 5982-5650) is added, 2min is subjected to vortex extraction, 5000 revolutions per minute is centrifuged for 3 minutes, 4mL of supernatant (methanol layer) is sucked into a QuEChERS purifying reagent tube (Part No:5982-4956 CH), 30s is subjected to vortex, 3000 revolutions per minute is centrifuged for 3 minutes, 1.0mL of the sample is taken into a nitrogen blowing tube, nitrogen is dried at 45 ℃, 1.0mL of acetic acid-methanol (8+2, volume ratio) mixed solution is accurately added for dissolution, and a 0.45 mu m organic phase filter membrane is adopted for filtration to be detected.
S2, sample detection:
LC-MS/MS liquid phase conditions
Chromatographic column:
BEHC18; column temperature: room temperature; sample injection amount: 5. Mu.L; the mobile phase and gradient elution conditions were as follows: />
LC-MS/MS Mass Spectrometry Condition
Adopts an ionization mode: ESI (electronic service provider interface) + And ESI (electronic service interface) - A mode; capillary voltage: 2.83kV; ion source temperature: 150 ℃; desolventizing gas temperature: 500 ℃; desolventizing gas flow: 800L/hr; MRM monitoring mode; collision gas: helium gas. The mass spectrometry conditions were as follows:
note that: * To quantify ions
S3, analyzing results: in ionization mode ESI + And ESI (electronic service interface) - And (3) performing full scanning on the standard solution in a mode to obtain molecular ions of a standard substance, performing secondary mass spectrometry on the molecular ions, selecting two characteristic fragment ions with larger signal intensity and stable signal, selecting the quantitative ion with the strongest relative abundance and the qualitative ion with the weaker relative abundance, drawing a standard curve, and quantifying the sample by an external standard method.
The present invention is not limited to the preferred embodiments, and the patent protection scope of the invention is defined by the claims, and all equivalent structural changes made by the application of the present invention are included in the scope of the invention.
Claims (5)
1. The detection method for simultaneously detecting 16 antibacterial and mildew-proof agents in bamboo products is characterized by comprising the following steps of:
s1, sample pretreatment: sample treatment is carried out by adopting a QuEhERS method or a solid-phase extraction method;
the QuEhERS method is adopted: weighing 1g of sample, adding 5mL of water into a 50mL plastic centrifuge tube, accurately adding 10.0mL of methanol, covering a cover, shaking uniformly, performing ultrasonic extraction for 30 minutes, adding a QuEChERS Extract Tubes EN Method extraction reagent pack, performing vortex extraction for 2min, performing centrifugation for 3 minutes at 5000 rpm, sucking 4mL of supernatant, placing the supernatant into a QuEChERS purification reagent tube, performing vortex 30s, performing centrifugation for 3 minutes at 3000 rpm, taking 1.0mL of the supernatant into a nitrogen blowing tube, performing nitrogen blow-drying at 45 ℃, accurately adding 1.0mL of acetic acid-methanol mixed solution for dissolution, filtering with a 0.45 mu m organic phase filter membrane, and performing test;
the solid phase extraction method comprises the following steps: weighing 1g of sample, adding 10mL of methanol-water solution containing 0.1% formic acid into a 50mL plastic centrifuge tube, covering a cover, shaking uniformly, performing ultrasonic extraction for 30 minutes, centrifuging at 5000 rpm for 3 minutes, taking 1.0mL of clear liquid, adding 1mL of water into the centrifuge tube, diluting, purifying by using an oasis MCX solid phase extraction column, controlling the column passing speed to be 1 drop/second, washing the extraction column by using 3mL of water and 3mL of methanol after the sample liquid passes through the column, performing vacuum pumping, eluting by using 10mL of 5% ammonia water-methanol solution, collecting eluent, drying by nitrogen at 45 ℃, accurately adding 1.0mL of acetic acid-methanol mixed solution for dissolution, filtering by using a 0.45 mu m organic phase filter membrane, and testing;
s2, sample detection: the sample extracting solution is detected by adopting ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry, and the detection conditions are as follows:
LC-MS/MS liquid phase conditions: comprises a chromatographic column: ACQUITY UPLC BEH C18; the mobile phase A is acetonitrile, the mobile phase B is acetic acid, and the mobile phase A contains 0.1% formic acid aqueous solution, and the column temperature is as follows: room temperature;
LC-MS/MS mass spectrometry conditions: ionization mode: esi+ and ESI-; capillary voltage: 2.83kV; ion source temperature: 150 ℃; desolventizing gas temperature: 500 ℃; desolventizing gas flow: 800L/hr; scanning mode: MRM mode; collision gas: helium gas;
s3, analyzing results: carrying out full scanning on the standard solution in ionization modes ESI+ and ESI-to obtain molecular ions of a standard substance, then carrying out secondary mass spectrometry on the molecular ions, selecting two characteristic fragment ions with larger signal intensity and stable signal, selecting the ion with the strongest relative abundance as a quantitative ion and the weaker ion as a qualitative ion, and drawing a standard curve to quantitatively determine a sample by an external standard method;
wherein the 16 antibacterial mildew preventive are benzoic acid, dimethyl fumarate, methyl parahydroxybenzoate, ethyl parahydroxybenzoate, propyl parahydroxybenzoate, butyl parahydroxybenzoate, salicylanilide, o-phenylphenol, carbendazim, thiabendazole, 3-iodo-2-propylbutylcarbamate, tebuconazole, didecyldimethylammonium chloride, imazalil, pentachlorophenol and natamycin;
the gradient elution conditions of the mobile phase in the LC-MS/MS liquid phase condition are as follows:
wherein, the mobile phase A and the mobile phase B are mixed according to volume percentage.
2. The method according to claim 1, wherein in step S1, after the nitrogen is blown dry, acetic acid and methanol are added to the mixed solution of acetic acid and methanol in a volume ratio of 8:2.
3. The method according to claim 1, wherein the solid phase extraction method is performed with a methanol-water solution containing 0.1% formic acid, and the volume ratio of methanol to water containing 0.1% formic acid is 1:1.
4. The method according to claim 1, wherein the sample injection amount in the step S2 is 5 μl.
5. The method of claim 1, wherein the mass spectrometry conditions for each of the antimicrobial and mildewcide agents are as follows:
and is a quantitative ion.
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