CN113156026A - Method for simultaneously measuring residual quantity of 18 plant growth regulators in bean sprouts - Google Patents
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for simultaneously determining the residual quantity of 18 plant growth regulators in bean sprouts, which takes the bean sprouts as a test raw material, a sample is treated by a QuEChERS method, then is extracted by a solution containing 5% acetic acid-acetonitrile (1:99, V/V), a dispersed solid phase extraction adsorbent is purified, a methanol solvent is converted to constant volume, then is filtered by a 0.22 mu m filter membrane, a Phenomenex H18 chromatographic column is selected for separation, qualitative analysis is carried out through retention time matching and the accurate mass quantity of parent ions and main fragment ions, and the quantity is determined by a matrix standard solution external standard method. Under optimized conditions, the retention time of 18 PGRs is 5.8-11.7 min. When the mass concentration range is between 0.005 mu g/mL and 0.05 mu g/mL, the linear relation of various PGRs is good, the correlation coefficient (r) is more than or equal to 0.9990, the method detection limit (S/N is 3) is between 0.03 mu g/kg and 0.92 mu g/kg, the quantification limit is between 0.50 mu g/kg and 2.10 mu g/kg, the normalized average recovery rate is between 85 and 110 percent on 3 concentration levels, and the relative standard deviation (N is 6) is between 2.8 and 7.5 percent. The method is simple and accurate to operate, and can be used for quickly, qualitatively and quantitatively analyzing the residues of the 18 PGRs in the bean sprouts.
Description
Technical Field
The invention relates to the technical field of methods for measuring the residual quantity of 18 plant growth regulators in bean sprouts, in particular to a method for measuring the residual quantity of 18 plant growth regulators in bean sprouts simultaneously.
Background
Plant Growth Regulators (PGRs) are substances having similar physiological and biological effects to phytohormones, also called phytohormones or Plant endogenous hormones, and can affect and effectively regulate the Growth and development of plants, including a series of Plant life processes from cell Growth, division, rooting, germination, flowering, fructification, maturation and abscission. In recent years, the phenomenon of abuse and improper use of PGRs sometimes occurs, which affects the edible safety of agricultural products and poses a threat to the health of people [1-5 ]. The 11-year-2015 publication issued by the former national food and drug administration, former Ministry of agriculture and former national institutes of health and family planning states mandates that the use of growth regulators such as 6-benzyladenine, 4-chlorophenoxyacetic acid and gibberellin in bean sprouts is prohibited. Therefore, developing a new technology for rapidly detecting the plant growth regulator residue in the bean sprouts has very important practical significance for ensuring food safety and promoting national health and social and economic development.
The basic research of the multi-residue detection technology and related limit standards of the plant growth regulator in China is still in the initial stage, and the national standard for simultaneously detecting the multi-residue is not established. At present, the methods for detecting the residue of plant growth regulators mainly include enzyme-linked immunosorbent assay (ELISA) 6, Gas Chromatography (GC) 7, gas chromatography-tandem mass spectrometry (GC-MS/MS) 8, High Performance Liquid Chromatography (HPLC) 9, liquid chromatography-mass spectrometry (LC-MS) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) 10. GC and GC-MS/MS need chemical derivatization, and the operation is more complicated. ELISA sensitivity is low, and trace analysis is difficult to realize. The sensitivity of HPLC is low, the influence of matrix interference is large, the pretreatment is complex and false positive interference is easily caused.
Disclosure of Invention
In order to solve the problems of difficult detection, low sensitivity and the like of the residual quantity of the plant growth regulators in the conventional bean sprouts, the invention aims to provide the method for simultaneously determining the residual quantity of the 18 plant growth regulators in the bean sprouts. The method has the advantages of simple operation, high sensitivity, good reproducibility, and accuracy meeting the methodological index, and can be used for simultaneously measuring the residual amounts of 18 PGRs in bean sprouts.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for simultaneously measuring the residual quantity of 18 plant growth regulators in bean sprouts is disclosed, wherein the 18 plant growth regulators are as follows: forchlorfenuron, gibberellic acid, cyclanilide, abscisic acid, indolypropionic acid, indoleacetic acid, p-chlorophenoxyacetic acid, thidiazuron, 6-benzylaminopurine, 4-iodophenoxyacetic acid, imazalil, 2,4-D, naphthylacetic acid, uniconazole, trinexamine, paclobutrazol, indolebutyric acid and trinexapac-ethyl; c18, graphitized carbon black, and N-propylethylenediamine were obtained from Shanghai spectral Co; methanol, formic acid, acetonitrile, NH4 AC; anhydrous magnesium sulfate, sodium chloride, acetic acid; the method is characterized by comprising the following steps:
(1) sample pretreatment: weighing 5.0g of bean sprout sample in an outer tube of a centrifuge tube, adding a mixed standard solution, standing for 30min, adding 10mL of 5% acetic acid-acetonitrile (1:99, V/V), adding an extraction salt package and 10 zirconium beads, screwing down an inner tube, putting the inner tube into an automatic QuEChERS pretreatment instrument for treatment, after 25min alternate oscillation and centrifugation, accurately absorbing 1.0mL of nitrogen of a supernatant to be blown to be dry, fixing the volume with 10% of methanol solution, and measuring a filtrate by using an organic microporous filter membrane of 0.22 mu m;
(2) and (3) detection: the standard working solution and the sample solution were injected under the following set chromatographic and mass spectrometric conditions:
chromatographic conditions are as follows: a chromatographic column: phenomenex H18(50 mm. times.3.00 mm, 2.60 μm); the sample injection volume is 5 mu L; column temperature: 35 ℃; mobile phase: a is a 5mmol/L ammonium acetate solution containing 0.1% formic acid, and B is methanol. Gradient elution: 0.5-5.0 min, 10% B; 5.0-8.0 min, 95% B; 8.0-12 min, 10% B; flow rate: 0.25 ml/min;
mass spectrum conditions: electrospray ion source (ESI), positive (ESI +), negative (ESI-) ion scan mode; the flow rate of the atomized gas is 3.00L/min; the flow rate of the drying gas is 15.00L/min; the temperature of the DL pipe is 250 ℃; electrospray voltage (IS): 2500V; the scanning time is 0.1 s; multiple reaction monitoring mode (MRM);
(3) preparing a standard solution: accurately sucking 100 mu L of single PGR standard substance with concentration of 1000 mu g/mL respectively, metering the volume to 10mL by using methanol to obtain mixed standard stock solution with concentration of 10 mu g/mL, and storing in a refrigerator at 4 ℃;
preparing 0.005 mu g/mL, 0.01 mu g/mL, 0.02 mu g/mL, 0.04 mu g/mL and 0.05 mu g/mL of matrix mixed standard working solution by using the blank solution of the sample, and preparing the standard working solution in situ
Preferably, in the above method for simultaneously measuring the residual amount of 18 plant growth regulators in bean sprouts, the salt comprises 5.5g of anhydrous magnesium sulfate, 1.5g of sodium chloride, 0.5g of disodium hydrogen citrate, and 1.0g of sodium citrate.
Preferably, in the above method for simultaneously measuring the residual amount of 18 plant growth regulators in bean sprouts, the inner tube contains 5 zirconia beads of 4mm, 200mg PSA, 500mg anhydrous magnesium sulfate, and 100mg C18。
According to the technical scheme, compared with the prior art, the invention has the following characteristics:
1) a method for simultaneously measuring the residual quantity of the 18 plant growth regulators in the bean sprouts is developed for the first time, and the technical blank is filled;
2) provides the optimal condition for simultaneously determining the residual quantity of the 18 plant growth regulators in the bean sprouts by the QuEChERS-high performance liquid chromatography-tandem mass spectrometry.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Figure 1 is a graph showing the recovery (n-3) of the plant growth regulator 18 of the present invention in different decontamination combinations.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The specific embodiment is as follows:
1 materials and methods
1.1 instruments and reagents
Agilent 6460 type HPLC-MS/MS, Agilent technologies (China) Inc.; 099ADPM12 model vortex mixer, Shanghai easily-expandable instruments Limited; model 3-15 high speed centrifuge, Hettich, Germany; EVA model 50A nitrogen blower, organization Associates, USA; a T-200 electronic balance, a Normal-maturing Shuangjie Instrument manufacturing plant; SZ13022-NY 0.22 μm organic filter membrane, Navigator laboratories Inc.
Standards for 18 PGRs: forchlorfenuron, gibberellic acid, cyclanilide, abscisic acid, indolypropionic acid, indoleacetic acid, p-chlorophenoxyacetic acid, thidiazuron, 6-benzylaminopurine, 4-iodophenoxyacetic acid, imazalil, 2,4-D, naphthylacetic acid, uniconazole, trinexamine, paclobutrazol, indolebutyric acid and trinexapac-ethyl (the purity is more than or equal to 99.0 percent, and the national standard substance center); c18Graphitized Carbon Black (GCB) and N-propyl ethylene diamine (PSA) were all available from Shanghai' an spectral Co; methanol, formic acid, acetonitrile, NH4AC (chromatographically pure, ASC corporation, usa); anhydrous magnesium sulfate, sodium chloride, acetic acid (analytical grade, Shanghai national pharmaceutical chemicals Co., Ltd.).
1.2 test methods
1.2.1 chromatographic conditions
A chromatographic column: phenomenex H18(50 mm. times.3.00 mm, 2.60 μm); the sample injection volume is 5 mu L; column temperature: 35 ℃; mobile phase: a is a 5mmol/L ammonium acetate solution containing 0.1% formic acid, and B is methanol. Gradient elution: 0.5-5.0 min, 10% B; 5.0-8.0 min, 95% B; 8.0-12 min, 10% B; flow rate: 0.25 ml/min.
1.2.2 Mass Spectrometry conditions
Electrospray ion source (ESI), positive (ESI +), negative (ESI-) ion scan mode; the flow rate of the atomized gas is 3.00L/min; the flow rate of the drying gas is 15.00L/min; the temperature of the DL pipe is 250 ℃; electrospray voltage (IS): 2500V; the scanning time is 0.1 s; multiple reaction monitoring mode (MRM).
1.2.3 preparation of Standard solution
Accurately sucking 100 μ L of single PGR standard substance with concentration of 1000 μ g/mL respectively, diluting to 10mL with methanol to obtain mixed standard stock solution with concentration of 10 μ g/mL, and storing in refrigerator at 4 deg.C. The blank solution of the sample is prepared into matrix mixed standard working solution of 0.005 mu g/mL, 0.01 mu g/mL, 0.02 mu g/mL, 0.04 mu g/mL and 0.05 mu g/mL respectively, and the working solution is prepared in situ.
1.2.4 sample pretreatment
Weighing 5.0g of bean sprout sample in an outer tube of a centrifuge tube, adding a mixed standard solution (external standard method), standing for 30min, adding 10mL of 5% acetic acid-acetonitrile (1:99, V/V), adding an extraction salt bag (containing 5.5g of anhydrous magnesium sulfate, 1.5g of sodium chloride, 0.5g of disodium hydrogen citrate and 1.0g of sodium citrate) and 10 zirconium beads, screwing an inner tube (containing 5mm of zirconium oxide beads, 200mg of PSA, 500mg of anhydrous magnesium sulfate and 100mg of C18), putting the inner tube into an automatic QuEChERS pretreatment instrument for starting treatment, after 25min alternate shaking and centrifugation, accurately absorbing 1.0mL of nitrogen of supernatant liquid to be blown to the near dry, using 10% methanol solution to fix the volume by an organic microporous filter membrane of 0.22 mu m, and supplying the filtrate for HPLC-MS/MS determination.
2 results and analysis
2.1 optimization of Mass Spectrometry conditions
1000 mug/L of 18 PGRs standard solutions are respectively injected into a mass spectrum system through a needle pump for parameter optimization. And (3) carrying out full scanning in a positive ion mode and a negative ion mode, wherein the scanning range m/z is 50-500, and primary mass spectrograms of 18 PGRs are obtained. Since the 18 PGRs have different properties and different ionization patterns, the ionization pattern is determined to be suitable for achieving the highest ionization effect. The ion with the highest response is selected as an excimer ion, the declustering voltage (DP) is optimized to obtain the strongest parent ion signal, two ions with stronger responses are selected as a quantitative ion and a qualitative ion, and the Collision Energy (CE) is optimized in a Multiple Reaction Monitoring (MRM) mode. The mass spectral parameters are shown in table 1.
Tables 1-18 Mass Spectrometry parameters of plant growth regulators, Note: the others are qualitative ions.
2.2 optimization of chromatographic conditions
The results of experiments comparing the separation effect of Phenomenex H18 chromatographic column (50mm multiplied by 3.00mm, 2.60 μm), Zorbax SB-C18 chromatographic column (100mm multiplied by 2.1m, 3.5 μm) and Waters Acquity BEH C18(50mm multiplied by 2.1mm, 7.0 μm) on the analyte show that the separation effect and peak shape of 18 PGRs on the Phenomenex H18 chromatographic column are the best. Thus, the Phenomenex H18 column was selected for analysis of the analyte in this experiment.
The experiment compares the separation effects of acetonitrile-water and methanol-water as mobile phases, and inspects the elution effect of the mobile phases on 18 PGRs, and the result shows that when the methanol-water is used as the mobile phase, the retention time of 18 objects to be detected on a chromatographic column is shortest, the separation effect and the peak shape are better, and the objects to be detected have higher response value and sensitivity when the methanol is used as an organic phase. Experiments show that formic acid is added into the mobile phase to ionize the object to be detected, and ammonium acetate has a promoting effect on the ionization effect of the target object in the negative ion mode. Respectively preparing 0.1% formic acid-1 mmol/L ammonium acetate-methanol with concentration (1); (2) 0.1% formic acid-5 mmol/L ammonium acetate-methanol; (3) 0.1% formic acid-10 mmol/L ammonium acetate-methanol; (4) the mobile phase of 0.3% formic acid-5 mmol/L ammonium acetate-methanol shows that the response and peak shape of each target object are optimal when 0.1% formic acid-5 mmol/L ammonium acetate-methanol is used as the mobile phase. Under the optimal elution condition, the retention time of the 18 PGEs is between 5.8 and 11.7 min.
2.3 optimization of purification conditions
The dispersive solid phase extraction technology (QuEChERS: Quick, Easy, Cheap, Effective, Rugged, Safe) is a rapid sample pretreatment technology for detecting agricultural products which is newly developed internationally in recent years, and matrix interference components are reserved mainly through polar interaction, nonpolar interaction, ionic interaction and other modes to achieve the purification effect. The main adsorption materials at present comprise Graphitized Carbon Black (GCB), N-propyl ethylenediamine (PSA) and C18, wherein the PSA mainly has a strong adsorption effect on polar substances and removes substances such as organic acids, pigments, metal ions, phenols and the like; GCB can effectively remove pigments; c18 has strong adsorption effect on nonpolar substances. A standard concentration of 50. mu.g/L was selected for the experiment and (1)100mg C18+25mg GCB +500mg MgSO4 was examined; (2)100mg C18+200mg PSA +500mg MgSO 4; (3)25mg GCB +200mg PSA +500mg MgSO 4; (4) the purification effect and recovery normalized to the standard under the conditions of 100mg C18+200mg PSA +25mg GCB +500mg MgSO44 are shown in FIG. 1. When 100mg of C18+200mg of PSA +500mg of MgSO4 is used as a purifying agent, the recovery rate of 18 PGRs is between 80% and 115%, so that 100mg of C18+200mg of PSA +500mg of MgSO4 is used as an adsorbent for sample purification in the experiment.
2.4 methodological validation
2.4.1 Linear Range, detection Limit and quantification Limit
The matrix effect is a common interference factor, which means that the matrix of the co-extraction of the sample can affect the ionization of the target substance, and the generated co-extraction has matrix enhancement or inhibition effect, and can be reduced or eliminated by adopting a proper method, so that the measurement accuracy and precision can be improved. The test takes a bean sprout sample without a target object as a blank matrix, and adopts a blank matrix solution to prepare a standard solution so as to eliminate the influence of the matrix effect. Taking a series of matrix standard solutions with mass concentrations of 0.005 mu g/mL, 0.01 mu g/mL, 0.02 mu g/mL, 0.04 mu g/mL and 0.05 mu g/mL respectively, drawing a standard curve by taking the mass concentration as an abscissa and taking a peak area as an ordinate, wherein a linear regression equation and a correlation coefficient are shown in a table 2. The results show that 18 PGRs have good linear relation in the concentration range of 0.005 mu g/mL-0.05 mu g/mL, and the correlation coefficients (r) are all more than or equal to 0.9990. The detection Limit (LOD) was calculated by a 3-fold signal-to-noise ratio (S/N ═ 3) method and the quantification Limit (LOQ) was calculated by a 10-fold signal-to-noise ratio (S/N ═ 10) method, and the results showed that LOD of 18 PGRs was 0.3 μ g/kg to 1.2 μ g/kg and LOQ was 1.0 μ g/kg to 5.0 μ g/kg (table 2).
Tables 2-18 Linear relationships, correlation coefficients, detection limits and quantitation limits for PGRs.
2.4.2 recovery and precision of Process
Using 5.0g of bean sprout samples containing no objective component as a blank substrate, 18 kinds of PGRs standards were added to prepare 3 portions of each of samples added at concentration levels of 10. mu.g/kg, 100. mu.g/kg and 200. mu.g/kg, and the measurement was repeated 6 times per concentration level to calculate the Relative Standard Deviation (RSD) of the measured values. As can be seen from Table 3, the average recovery of each additive concentration level was 85% -110%, the RSD was 2.8% -7.5%, and the accuracy and precision of the method both met the requirements of the residual analysis.
Table 3-18 PGRs addition recovery and precision (n ═ 6).
2.5 actual sample analysis
Detecting 30 batches of bean sprout samples randomly purchased in the market by using the established analysis method, wherein 4-chlorophenoxyacetic acid (4-CPA) is detected in 3 batches of the detected samples, and the content of the 4-chlorophenoxyacetic acid is lower than the quantitative limit; 6-benzyladenine (6-BA) is detected from 2 batches of samples, the content is respectively 2.4 mu g/kg and 10.6 mu g/kg, and the samples are unqualified samples. None of the other 16 PGRs were detected.
3 conclusion
In the experiment, 5% acetic acid-acetonitrile (1:99, V/V) is used as an extraction solvent, a sample is purified by a QuEChERS method, and a HPLC-MS/MS simultaneous determination method of 18 PGRs in bean sprouts is established by optimizing chromatographic and mass spectrum conditions. The method has the advantages of simple operation, high sensitivity, good reproducibility, and accuracy meeting the methodological index, and can be used for simultaneously measuring the residual amounts of 18 PGRs in bean sprouts.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. A method for simultaneously measuring the residual quantity of 18 plant growth regulators in bean sprouts is disclosed, wherein the 18 plant growth regulators are as follows: forchlorfenuron, gibberellic acid, cyclanilide, abscisic acid, indolypropionic acid, indoleacetic acid, p-chlorophenoxyacetic acid, thidiazuron, 6-benzylaminopurine, 4-iodophenoxyacetic acid, imazalil, 2,4-D, naphthylacetic acid, uniconazole, trinexamine, paclobutrazol, indolebutyric acid and trinexapac-ethyl; c18, graphitized carbon black, and N-propylethylenediamine were obtained from Shanghai spectral Co; methanol, formic acid, acetonitrile, NH4 AC; anhydrous magnesium sulfate, sodium chloride, acetic acid; the method is characterized by comprising the following steps:
(1) sample pretreatment: weighing 5.0g of bean sprout sample in an outer tube of a centrifuge tube, adding a mixed standard solution, standing for 30min, adding 10mL of 5% acetic acid-acetonitrile (1:99, V/V), adding an extraction salt package and 10 zirconium beads, screwing down an inner tube, putting the inner tube into an automatic QuEChERS pretreatment instrument for treatment, after 25min alternate oscillation and centrifugation, accurately absorbing 1.0mL of nitrogen of a supernatant to be blown to be dry, fixing the volume with 10% of methanol solution, and measuring a filtrate by using an organic microporous filter membrane of 0.22 mu m;
(2) and (3) detection: the standard working solution and the sample solution were injected under the following set chromatographic and mass spectrometric conditions:
chromatographic conditions are as follows: a chromatographic column: phenomenex H18(50 mm. times.3.00 mm, 2.60 μm); the sample injection volume is 5 mu L; column temperature: 35 ℃; mobile phase: a is a 5mmol/L ammonium acetate solution containing 0.1% formic acid, and B is methanol. Gradient elution: 0.5-5.0 min, 10% B; 5.0-8.0 min, 95% B; 8.0-12 min, 10% B; flow rate: 0.25 ml/min;
mass spectrum conditions: electrospray ion source (ESI), positive (ESI +), negative (ESI-) ion scan mode; the flow rate of the atomized gas is 3.00L/min; the flow rate of the drying gas is 15.00L/min; the temperature of the DL pipe is 250 ℃; electrospray voltage (IS): 2500V; the scanning time is 0.1 s; multiple reaction monitoring mode (MRM);
(3) preparing a standard solution: accurately sucking 100 mu L of single PGR standard substance with concentration of 1000 mu g/mL respectively, metering the volume to 10mL by using methanol to obtain mixed standard stock solution with concentration of 10 mu g/mL, and storing in a refrigerator at 4 ℃;
the blank solution of the sample is prepared into matrix mixed standard working solution of 0.005 mu g/mL, 0.01 mu g/mL, 0.02 mu g/mL, 0.04 mu g/mL and 0.05 mu g/mL respectively, and the working solution is prepared in situ.
2. The method for simultaneously measuring the residual amount of 18 plant growth regulators in bean sprouts according to claim 1, wherein the salt comprises 5.5g of anhydrous magnesium sulfate, 1.5g of sodium chloride, 0.5g of disodium hydrogen citrate and 1.0g of sodium citrate.
3. The method for simultaneously measuring the residual amount of 18 plant growth regulators in bean sprouts according to claim 1, wherein the inner tube contains 5 zirconia beads with a diameter of 4mm, 200mg PSA, 500mg anhydrous magnesium sulfate and 100mg C18。
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