CN105445360A - Method for quickly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography) - Google Patents
Method for quickly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography) Download PDFInfo
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Abstract
The invention belongs to the technical field of detection and discloses a method for directly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography). The method comprises steps as follows: (1) m/z 221, 223 and 225 ion peaks produced due to the dichlorvos C1 atom isotope effect in the mass spectrography are presented; (2) m/z 223 is selected as primary characteristic ions of the dichlorvos for splitting, and secondary ions m/z 127 are used for quantitative analysis; (3) structural analysis is performed on secondary characteristic ions m/z 109, 127, 145 and 147 of dichlorvos m/z 223; (4) a 50 mL conical flask is selected to contain 20 mL of the honey, and the condition that the honey is blown to pollute or block a pipeline during desorption is effectively prevented. According to the method, a to-be-tested sample is not required to be pretreated, the influence of complex matrixes in the honey can be borne, and the dichlorvos in the honey is directly and quickly detected.
Description
Technical field
The invention belongs to detection technique field, particularly the detection method of DDVP in honey.
Background technology
China is the first in the world bee-keeping big country, is also that bee product is produced and big export country.Honey is the natural food that a kind of nutritive value is very high, containing the multiple nutrients material required for body metabolism, has bowl spares simultaneously, moisturizes, the effect of pain relieving and suppression and sterilization.But the problems such as microbial contamination in honey, metallic pollution, residues of pesticides and microbiotic pollution bring great hidden danger to the health of honey market and the mankind.DDVP (Dichlorvos, DDVP) is a kind of pesticide of wide spectrum, cheap and good drug efficacy, due to beekeeper's abuse DDVP when treating bee colony and nectariferous plant disease and pest, causes that DDVP in honey is residual to exceed standard.Along with global economic integration and food trade internationalization, in honey, DDVP remains and is subject to the special concern of Main Economic body as European Union, the U.S. and Japan and other countries and area, and examination criteria is further harsh, has a strong impact on the development in honey market.
In current detection honey, the main method of DDVP has gas chromatographic technique, liquid chromatography-tandem mass spectrometry technology and gas chromatography tandem mass spectrometry technology.These detection methods need through the loaded down with trivial details sample pretreatment process such as solvent extraction, Solid-Phase Extraction, supercritical fluid extraction, have complex operation step, the defect such as time-consuming, the needs that can not meet directly, detect fast.
Summary of the invention
The object of this invention is to provide a kind of method DDVP in honey being remained to direct-detection newly.
The present invention, without the need under the condition of sample pretreatment, can carry out directly, fast detecting to the DDVP in honey.Adopt the two-stage tandem fragment of DDVP to carry out quantitative test, avoid false positive, substantially increase the accuracy of detection.
Detection method of the present invention carries out the detection of honey sample DDVP.
Concrete technical scheme is as follows:
A kind of method of DDVP in neutral desorption electrospray extraction MALDI-MS (ND-EESI-MS) direct-detection honey, comprises the following step:
(1) DDVP standard solution preparation: get DDVP standard items, be mixed with the storing solution of 400 μ g/mL with methyl alcohol, in 4 DEG C of stored refrigerated; Dilute storing solution with ultrapure water during experiment, be mixed with the DDVP standard items aqueous solution of 0.5-100 μ g/mL gradient concentration;
(2) accurate measuring 19.80mL not containing DDVP honey respectively in 50mL conical flask, preservative film seal, 45 DEG C of water-bath 5min; Add the DDVP standard items aqueous solution of 0.2mL gradient concentration in respectively filling not containing in the conical flask of DDVP honey, stir, cool to room temperature, obtains mark-on honey, carries out Mass Spectrometer Method;
The honey sample to be measured of accurate measuring 19.80mL is respectively in 50mL conical flask, and preservative film seals, 45 DEG C of water-bath 5min; Add 0.2mL ultrapure water, stir, treat honey cool to room temperature, carry out Mass Spectrometer Method;
(3) neutral desorption electrospray extraction MALDI-MS detects: ND-EESI-MS is set to positive ion detecting pattern, scanning of the mass spectrum scope m/z60 ~ 300; Neutral desorb spraying reagent is methyl alcohol: aqueous solution; Extractant is methyl alcohol: water: formic acid (V/V=2:2:1), flow velocity 5 μ L/min; Ionization voltage 3.8kV; Atomization gas pure nitrogen gas pressure is 1.2MPa; Sample end assist gas pressure is 1.2MPa; Ion transfer tube temperature is 200 DEG C; During collision induced dissociation experiment, DDVP parent ion isolation width is 1.1Da, and collision energy is 25%, and collision duration is 30ms; For ensureing that sample molecule carries out colliding and reacting with reagent ion to greatest extent, sample channel mouth and mass spectrum mouth horizontal sextant angle keep 150 °, two spray channel angles keep 60 °, and two spray channel mouths and mass spectrum mouth distance are 0.5cm, other parameter LTQ-MS system Automatic Optimal;
(4) qualitative analysis: if there is m/z109 and m/z127 ion signal peak in the secondary fragment of m/z223, illustrates in honey sample to be measured containing DDVP;
Quantitative test: select the secondary characteristics ion m/z127 of m/z223 to carry out quantitative test, with the concentration of DDVP in mark-on honey for horizontal ordinate, the clean response signal mean value of its m/z127 is ordinate drawing standard curve; According to typical curve, and the signal intensity of m/z223 secondary characteristics ion m/z127 in honey sample to be measured, draw the content of DDVP in honey sample to be measured.
Described neutral desorb spraying reagent methyl alcohol: water volume ratio 2:3 solution.
The invention has the beneficial effects as follows: (1) the present invention selects the secondary characteristics fragment m/z127 of DDVP one-level characteristic ion m/z223 to carry out quantitative test, to avoid false positive; (2) methyl alcohol is adopted: water: formic acid (V/V=2:2:1) is as extractant; Methyl alcohol: water (V/V=2:3) is neutral desorb reagent, make DDVP desorption efficiency in honey high, echo signal is strong; (3) without the need to preprocessing process such as dilutions, achieve the in-situ study of DDVP in honey, detect and be limited to 1.03ng/mL, far below the detection limit 15.567ng/mL that Chloramphenicol Residue in Honey detects; (4) application of the direct Fast Detection Technique of pollutant in honey is made to become possibility, for the sustainable development of honey industry lays the foundation.
Accompanying drawing explanation
Fig. 1 is the ND-EESI Experimental equipment of the inventive method.
Fig. 2 is DDVP of the present invention (500ng/mL) MS
nspectrogram, in figure, (a) is DDVP methanol solution EESI-MS
nmass spectrogram, (b) is mark-on honey DDVP ND-EESI-MS
nmass spectrogram.
Fig. 3 is DDVP secondary characteristics ion m/z127 change in signal strength in extractant Optimal Experimental of the present invention, figure (a) is for different organic solvents is as extractant, b () is for adding different volumes (1% in methanol/water, 5%, 10%, 15%, 20%) formic acid and acetic acid are as extractant.
Fig. 4 is different proportion methanol/water (V/V=10:0,4:1,3:2,1:1 of the present invention; 2:3,1:4; 0:10) as neutral strippant m/z127 change in signal strength.
Fig. 5 is the optimization figure affecting DDVP mass spectrum behavior condition in the present invention, in figure, a () is electron spray voltage optimization figure, b () is extractant flowing rate figure, c () is atomization gas pressure optimization figure, d () is sample end assist gas pressure optimization figure, (e) is ion transfer tube temperature optimization figure.
Fig. 6 is the working curve of variable concentrations mark-on honey.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
The LTQ-XL Linear ion trap mass spectrometer that the mass spectrometer that example of the present invention uses is Finnigan company of the U.S., data handling system is the Xcalibur data handling system of Finnigan company of the U.S..
Neutral desorption apparatus and EESI ion gun, developed voluntarily by Jiangxi Province's mass spectrum science and instrument key lab; Precision electronic balance (METTLERTOLEDO).Methyl alcohol (chromatographically pure, TEDIA company of the U.S.); DDVP standard items (purity is 98.8%, lark prestige Science and Technology Ltd.);
This experiment uses the ND-EESI-MS method shown in Fig. 1 to test DDVP methyl alcohol standard solution (400ng/mL), and result as shown in Figure 2.DDVP molecule contains two chlorine atoms, reflects isotope rule in spectrogram, and in the positive-ion mode, m/z221, m/z223, m/z225 quasi-molecular ions (as Fig. 2 (b)) appears in one-level spectrogram.For avoiding false positive, selecting m/z223 to be that parent ion carries out second mass analysis, obtaining fragments characteristic ion m/z109, m/z127, m/z145 and m/z147, be respectively parent ion and lose (C
2hOCl
2), (C
2hCl
2), (C
2hO
37and (C Cl)
2hO
35cl) obtain, consistent with the fragments characteristic in document.For guaranteeing experimental reliability, EESI-MS is adopted to carry out MS/MS mass spectrum check analysis to 400ng/mL DDVP standard solution.Result shows, DDVP ND-EESI-MS
nspectrogram and its EESI-MS
nspectrogram fits like a glove.Therefore, if signal peak m/z223 can be detected in actual sample, and in MS/MS spectrogram, observe principal character ion m/z109 and m/z127, then can judge in this sample containing DDVP.
For getting rid of false positive when detecting, DDVP secondary characteristics ion m/z127 is adopted to be echo signal, for improving its signal intensity, the optimization of extractant has been carried out in this experiment, with the DDVP mark-on honey of 400ng/mL for experimental subjects, carry out the Optimal Experimental of methanol/water, water, methyl alcohol, ethanol, acetone, acetonitrile, benzene, dimethylbenzene and ethyl acetate, the variation tendency of research second order ms m/z127 signal intensity.Result shows: wherein using acetone, acetonitrile, benzene, dimethylbenzene and ethyl acetate as extractant, DDVP secondary characteristics ion m/z127 signal intensity is 0-2; Under other extractants, DDVP secondary characteristics ion m/z127 signal intensity is as Fig. 3 (a).Methanol/water is adopted to add the formic acid of different volumes mark (1%, 5%, 10%, 15%, 20%) or acetic acid (mass spectrometer allows maximal acid concentration 20%) as extractant, record m/z127 signal intensity.Result as Fig. 3 (b), adding 20% formic acid and methyl alcohol: water: when formic acid (V/V=2:2:1) is as extractant, in honey, DDVP secondary characteristics ion m/z127 signal intensity is the highest.Namely this experiment optimum extractant is methyl alcohol: water: formic acid (V/V=2:2:1).
Neutral strippant optimization is carried out in this experiment, with methyl alcohol: water: formic acid (V/V=2:2:1) is extractant, successively by methyl alcohol, methyl alcohol: water (V/V=4:1), methyl alcohol: water (V/V=3:2), methyl alcohol: water (V/V=1:1), methyl alcohol: water (V/V=2:3), methyl alcohol: water (V/V=1:4), water are that strippant detects DDVP secondary characteristics ion m/z127 signal intensity, result as shown in Figure 4, when neutral desorb reagent is methyl alcohol: time water (V/V=2:3), the signal intensity of secondary characteristics ion m/z127 is the highest.
The exploration of ion gun condition has been carried out in this experiment, and according to the mass spectrum behavior of DDVP standard solution, in the positive-ion mode, all the clean response signal intensity of selection DDVP secondary characteristics ion m/z127 represents the detection efficiency to DDVP molecule.As shown in Fig. 5 (a), during voltage too little (being less than 2kV), signal intensity is lower, along with the increase of voltage, Target Signal Strength raises rapidly, when voltage too large (being greater than 3.8kV), signal intensity decreases on the contrary, reaches best when 3.8kV; As shown in Fig. 5 (b), the extraction efficiency of extractant flow velocity when 5 μ L/min is maximum; As shown in Fig. 5 (c), experiment shows, along with the increase of atomization pressure, Target Signal Strength also increases thereupon, when air pressure exceedes certain value (being greater than 1.2MPa), major part ion can be buried in oblivion at mass spectrum mouth edge, and Target Signal Strength also can significantly decline, and reaches best when 1.2MPa; As shown in Fig. 5 (d), when sample end assist gas pressure is 1.2MPa, signal is the strongest, and desorption efficiency is the highest; As shown in Fig. 5 (e), temperature is from 100 DEG C ~ 200 DEG C, and Target Signal Strength raises rapidly, and when temperature is greater than 200 DEG C, signal intensity declines gradually, and therefore, experimental selection ion transfer tube temperature is 200 DEG C.
The experiment of mark-on honey DDVP is carried out, to determine the range of linearity and the detection limit of this method according to above-mentioned experimental technique and top condition.Owing to detecting in real time in honey sample, in order to get rid of false positive signal, the secondary characteristics ion m/z127 of experimental selection m/z223 carries out quantitative test, deducts corresponding blank background.The sample parallel of each concentration measures 6 times, with m/z127 clean response signal mean value and corresponding DDVP concentration drawing standard curve, as shown in Figure 6.Experiment shows, DDVP concentration is within the scope of 5 ~ 1000ng/mL, and linear relationship is good, and equation of linear regression is y=7.63x-13.82, R
2=0.998, according to the typical curve of gained mark-on DDVP, calculate the concentration of DDVP in testing sample.According to S/N=3, LOD=c3 σ/S, (c is the concentration of standard items, and σ is standard deviation, and S is net phase induction signal average strength), obtains detecting of mark-on honey and is limited to 1.03ng/mL.
In order to verify the credibility of this working curve, carry out recovery experiment.To concentration be 10 and 30 and the mark-on honey honey of 400ng/mL test, the mark-on honey replicate determination of each concentration 6 times, the recovery is respectively 93.01% (RSD is 4.37%), 96.03% (RSD is 3.30%) and 102.95% (RSD is 4.25%).
Embodiment 2
Commercially available honey preparation: the honey of accurate measuring 19.80mL is respectively in 50mL conical flask, and preservative film seals, 45 DEG C of water-bath 5min; Adding 0.2mL aqueous solution in respectively filling in the conical flask of honey, stirring; Treat honey cool to room temperature, carry out Mass Spectrometer Method;
Neutral desorption electrospray extraction MALDI-MS detects: ND-EESI-MS is set to positive ion detecting pattern, scanning of the mass spectrum scope m/z60 ~ 300; Neutral desorb spraying reagent methyl alcohol: water (V/V2:3); Extractant is methyl alcohol: water: formic acid (V/V2:2:1), flow velocity 5 μ L/min; Ionization voltage 3.8kV; Atomization gas (nitrogen, purity 99.999%) pressure is 1.2MPa; Sample end assist gas pressure is 1.2MPa; Ion transfer tube temperature is 200 DEG C.During collision induced dissociation experiment, DDVP parent ion isolation width is 1.1Da, and collision energy is 25%, and collision duration is 30ms; For ensureing that sample molecule carries out colliding and reacting with reagent ion to greatest extent, sample channel mouth and mass spectrum mouth horizontal sextant angle keep 150 °, two spray channel angles keep 60 °, and two spray channel mouths and mass spectrum mouth distance are 0.5cm, other parameter LTQ-MS system Automatic Optimal.
Qualitative analysis: if there is m/z109 and m/z127 ion signal peak in the secondary fragment of m/z223, containing DDVP in interpret sample;
Quantitative test: select the secondary characteristics ion m/z127 of m/z223 to carry out quantitative test, with the concentration of DDVP in mark-on honey for horizontal ordinate, the clean response signal mean value of its m/z127 is ordinate drawing standard curve; According to typical curve, and the signal intensity of m/z223 secondary characteristics ion m/z127 in honey sample to be measured, draw the content of DDVP in honey sample to be measured.
The commercially available honey testing result of table 1
Carry out ND-EESI-MS detection according to above-mentioned experimental technique to 9 commercially available honey samples, each sample parallel measures 6 times, and result is as shown in table 1.Result shows, and have 4 kinds of honey to detect containing DDVP, concentration is before 2.260 ~ 2.985ng/mL, and other 5 honey samples do not detect.Technical solution of the present invention lowest detection line can be low to moderate 1.03ng/mL, far below conventional method and conventional extraction agent detection line, has extraordinary Detection results.
Claims (2)
1. neutral desorption electrospray extracts a method for DDVP in MALDI-MS (ND-EESI-MS) direct-detection honey, it is characterized in that comprising the following step:
(1) DDVP standard solution preparation: get DDVP standard items, be mixed with the storing solution of 400 μ g/mL with methyl alcohol, in 4 DEG C of stored refrigerated; Dilute storing solution with ultrapure water during experiment, be mixed with the DDVP standard items aqueous solution of 0.5-100 μ g/mL gradient concentration;
(2) accurate measuring 19.80mL not containing DDVP honey respectively in 50mL conical flask, preservative film seal, 45 DEG C of water-bath 5min; Add the DDVP standard items aqueous solution of 0.2mL gradient concentration in respectively filling not containing in the conical flask of DDVP honey, stir, cool to room temperature, obtains mark-on honey, carries out neutral desorption electrospray extraction MALDI-MS and detects;
The honey sample to be measured of accurate measuring 19.80mL is respectively in 50mL conical flask, and preservative film seals, 45 DEG C of water-bath 5min; Add 0.2mL ultrapure water, stir, carry out neutral desorption electrospray extraction MALDI-MS and detect;
(3) neutral desorption electrospray extraction MALDI-MS detects: ND-EESI-MS is set to positive ion detecting pattern, scanning of the mass spectrum scope m/z60 ~ 300; Neutral desorb spraying reagent is methyl alcohol: aqueous solution; Extractant is methyl alcohol: water: formic acid (volume ratio 2:2:1), flow velocity 5 μ L/min; Ionization voltage 3.8kV; Atomization gas pure nitrogen gas pressure is 1.2MPa; Sample end assist gas pressure is 1.2MPa; Ion transfer tube temperature is 200 DEG C; During collision induced dissociation experiment, DDVP parent ion isolation width is 1.1Da, and collision energy is 25%, and collision duration is 30ms; For ensureing that sample molecule carries out colliding and reacting with reagent ion to greatest extent, sample channel mouth and mass spectrum mouth horizontal sextant angle keep 150 °, two spray channel angles keep 60 °, and two spray channel mouths and mass spectrum mouth distance are 0.5cm, other parameter LTQ-MS system Automatic Optimal;
(4) qualitative analysis: if there is m/z109 and m/z127 ion signal peak in the secondary fragment of m/z223, illustrates in honey sample to be measured containing DDVP;
Quantitative test: select the secondary characteristics ion m/z127 of m/z223 to carry out quantitative test, with the concentration of DDVP in mark-on honey for horizontal ordinate, the clean response signal mean value of its m/z127 is ordinate drawing standard curve; According to typical curve, and the signal intensity of m/z223 secondary characteristics ion m/z127 in honey sample to be measured, draw the content of DDVP in honey sample to be measured.
2. method according to claim 1, is characterized in that neutral desorb spraying reagent methyl alcohol: water volume ratio 2:3 solution.
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