CN101762663A - Preprocessing method for agricultural chemical multiresidue measurement in garlic samples - Google Patents
Preprocessing method for agricultural chemical multiresidue measurement in garlic samples Download PDFInfo
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Abstract
The invention relates to a preprocessing method for the agricultural chemical multiresidue measurement in garlic samples, which comprises the following steps of: choosing the microwave treatment as the preprocessing method for the garlic, and carrying out experiment on the influence of the microwave treatment time on the agricultural chemical stability; choosing the microwave oven to heat for 90 to 120 seconds, and inactivating the enzyme in the garlic sample before the garlicin production, which does not produce the garlicin, thereby removing the interference of the sulphide and enabling the recovery rate of the measurement and analysis needed object to meet the requirement. The measurement method of the invention has the characteristics of simple and fast operation, high recovery rate, high sensitivity and complete sulphide interference removing, and provides reliable guarantee for building a simple and effective analysis method and fast and accurately measuring the agricultural chemical residue in the garlic.
Description
Technical field:
The invention belongs to the pesticide residue determination technical field, relate to the method for Fast Determination of Pesticide Residue in the garlic.In particular, be to utilize microwave treatment to remove the gas chromatography method (GC/MS) of 205 kinds of residues of pesticides in the garlic.
Background technology:
Garlic is in planting process, and subterranean pest-insect harm is serious, makes the vegetable grower use high-toxic pesticide in a large number, and garlic is caused severe contamination.The agricultural chemicals phenomenon that exceeds standard is serious.In vegetable pesticide residue detected, sulfur-bearing vegetables such as onion, garlic and leek were the comparatively special complex samples of a class.When these class vegetables were blended in the specimen preparation process, organized enzyme wherein can make the sulfide in the vegetables discharge, and produces special odor.These sulfide are difficult for removing, and can produce very strong response on gas chromatography electron capture detector (GC/ECD), gas chromatographic flame photometric detector (GC/FPD) and gas chromatography mass detector (GC/MS), influence the qualitative and quantitative of determinand.Therefore solve that the interference of sulfide is the key of residues of pesticides in the gas chromatography determination sulfur-bearing vegetables in the sample.
Generally contain allicin in the garlic, allicin is that form with garlic aminoacid exists in fresh garlic, when garlic is subjected to impacting, big allinase touches airborne oxygen and is activated, garlic aminoacid generation enzymatic reaction changes into allicin, because the structure and the similar performance of allicin and some agricultural chemicals therefore carrying out can producing strong interference when pesticide multi-residues is analyzed, so the inactivation of allinnase are to eliminate the key that this class is disturbed.
General microwave treatment commonly used and phosphoric acid are handled, and the effect of microwave and phosphoric acid is to make organized enzyme inactivation in the sulfur-bearing vegetables, when chopping, just can not produce sulfide like this, have significantly reduced to measure and have disturbed.In addition, adopt silver nitrate to be distributed to the report of removing sulfide in the vegetables in aluminium oxide and the fluorine sieve on the tripoli in addition, but silver nitrate have very strong absorption to the sulfur-bearing agricultural chemicals, makes the recovery can not reach requirement.Also can remove sulfide in the vegetables with potassium permanganate-sulfuric acid oxidation method, but not be suitable for the unsettled organophosphorus insecticide of character.But adopt when adding copper sulphate homogenate method mensuration rape, rapeseed and beet sample, good effect is also arranged removing sulfide.
Summary of the invention:
The present invention has selected the pre-treatment means of microwave treatment as garlic, and microwave treatment time is tested the influence of agricultural chemicals stability.To put in order the direct microwave treatment of lobe garlic, before allicin produces, make the enzyme deactivation in the garlic samples, and also just can not produce allicin, thereby reach the interference of removing sulfide, and make the test analyte recovery reach requirement again.For achieving the above object, the invention provides following technical scheme:
The pre-treating method that pesticide multi-residues is measured in the garlic samples is characterized in that being undertaken by following step:
(1) garlic peeling, whole lobe claim 100-200g to use 500W microwave heating 90-120 second, and sample homogenization is handled;
(2) accurately take by weighing sample 10g (being accurate to 0.1g) and add 40-60mL acetonitrile and 10-20mL water, stir 2-5min with 20000-30000 commentaries on classics/min homogenate; The 5mL acetonitrile is washed cutter head, and suction filtration, 15-30mL acetonitrile divide the cleaning residue three times, and is behind the interpolation water 1-5mL, to be clean;
(3) with 10-20mL acetonitrile and 10-30mL pure water difference pre-leaching C18 post (1000mg represents the pillar specification), above-mentioned filtrate is crossed the PSA column purification, directly said extracted liquid is crossed post, (PSA wherein is a kind of solid-phase extraction column adopted name not need leacheate, concrete filler is the solid-phase extraction column of N-propyl group ethylenediamine, C18 is that filler is the solid-phase extraction column of three palaces energy octadecyl), use the 9-15mL acetonitrile, 3-5mL washes raffinate;
(4) eluent adds saturated 2mol/L phosphate buffer solution of 5mL salt and 6-10g salt, vibration 3-5min, static 10-15min;
(5) get upper solution, at 38 ℃ of following concentrating under reduced pressure; Concentrate is carried out the 2nd time purify, with eluent A 5mL pre-leaching, PSA post (500mg represents the pillar specification) is used 30mL eluent B wash-out then, uses 30mL eluent A wash-out again, collects eluent; Eluent A wherein: acetone+normal hexane (50mL+50mL); Eluent B: acetone+normal hexane (20mL+80mL).
(6) add decane 50 μ L in the eluent, closely dried at 38 ℃ of following concentrating under reduced pressure, dry up with Nitrogen evaporator, 2mL constant volume liquid { acetone+normal hexane (50mL+50mL) } constant volume is collected in the sample flasket, measures for GC/MS.
The concrete steps of the pre-treating method that pesticide multi-residues is measured in the garlic samples of the present invention are as follows:
1, test material and instrument and equipment
Reagent: except as otherwise herein provided, it is pure that reagent is analysis, and water is distilled water acetonitrile, acetone (chromatographically pure), normal hexane (chromatographically pure); Eluent A: acetone+normal hexane (50+50), eluent B: acetone+normal hexane (20+80), constant volume liquid: acetone+normal hexane (50+50); Sodium chloride; Decane; The pre-service pillar: the C18 post (500mg, 3mL), the PSA post; The 2mol/L phosphate buffer solution (pH=7.5) that salt is saturated; Standard sample of pesticide (purity all 〉=95%, available from German Dr.Ehrenstorfer company); Standard sample of pesticide stock solution: 200mg/L; Working stamndard solution: A:1000 μ g/L; B:500 μ g/L; C:50 μ g/L.
Instrument and equipment: Agilent6890/5973N gas chromatograph-mass spectrometer (GCMS): be furnished with electron bombardment ionization source (EI), electronic balance (100,000/, Switzerland Mei Tele company), micro-wave oven (Glanz), solid-phase extracting instrument (Japanese GLSciences), sample homogenization machine (IKA-WERKE), separating funnel oscillator (MMV-1000W) rotary evaporator (Laborota4000efficient, Germany Heidolph), automatic fast concentrating instrument (DSY-II type, elite garden technical institute of Beijing gold section) etc.
2, pre-treating method:
Take by weighing the garlic peeling, whole lobe claims 100g to heat 90 seconds with micro-wave oven (500W), and the sample homogenization machine is handled.Accurately take by weighing sample 10g (being accurate to 0.1g) in the 250mL beaker, add 40mL acetonitrile and 10mL water, the homogenate of homogeneous stirrer (20000 is changeed/min) 2min; The 5mL acetonitrile is washed cutter head, and suction filtration, 15mL acetonitrile divide the cleaning residue three times, and is behind the interpolation water 1mL, to be clean.
Purify: with 10mL acetonitrile and 10mL pure water difference pre-leaching C18 post (1000mg), above-mentioned filtrate is crossed column purification, use the 9mL acetonitrile, 3mL washes raffinate.Eluent is poured in the 500mL separating funnel, added saturated 2mol/L phosphate buffer solution of 5mL salt and 6.5g salt, vibration 3min, static 10min.Get the upper strata acetonitrile layer, at 38 ℃ of following concentrating under reduced pressure.
Concentrate is carried out 2 times purify,, use 30mL eluent B wash-out then, use 30mL eluent A wash-out again, collect eluent with eluent A 5mL pre-leaching PSA post (500mg).Add decane 50 μ L in the eluent, closely dried at 38 ℃ of following concentrating under reduced pressure, dry up 2mL constant volume liquid constant volume with Nitrogen evaporator.Be collected in the sample flasket, measure for GC/MS.
3, instrumental analysis condition
3.1 GC conditions
Injector temperature:
60 ℃, kept 0.1 minute, per minute rises to 260 ℃ for 150 ℃, keeps 3 minutes, rises to 300 ℃ with 40 ℃ of per minutes again, keeps 5 minutes;
Input mode:
Pulse is not shunted; Sampling volume: 2 μ L;
Chromatographic column:
HP-5ms(30m×0.25mm×0.251μm)。
Column temperature: 60 ℃, kept 3 minutes, per minute rises to 120 ℃ for 5 ℃, keeps 2 minutes, rises to 225 ℃ with 1.5 ℃ of per minutes again, keeps 2 minutes, and per minute rises to 300 ℃ for 20 ℃, keeps 10 minutes, moves 102.75 minutes altogether.
Carrier gas: He; Post flow: 1mL/min.
3.2 mass spectrum condition:
The EI source; Electron energy 70ev; Reaction gas: helium;
MS?Source：230℃；MS?Quad：150℃；Scan：50-500；
3.3 ion grouping situation
Table 1SIM method agricultural chemicals ion channel grouping sheet
| Sequence number | Time/min | Ion/amu | Residence time/ms |
| ??1 | ??10.00 | ??56，94，95，109，113，115，127，132，138，141，??157，164，185，191 | ??30 |
| ??2 | ??22.80 | ??55，77，83，93，107，113，120，121，122，125，126，??127，136，141，157，164，176，196，203，208，261 | ??30 |
| ??3 | ??34.60 | ??77，110，121，150，152，158，168，169，176，196，??203，242，261 | ??30 |
| ??4 | ??38.30 | ??55，78，91，111，121，125，127，129，135，150，??151，158，159，166，181，183，213，216，219，260，??264，276，292，306，316 | ??30 |
| ??5 | ??42.20 | ??54，57，118，124，125，137，143，149，164，176，??181，183，186，200，201，204，206，215，219，220，??221，229，231，237，246，262，288，295 | ??30 |
| ??6 | ??46.30 | ??57，109，127，137，145，147，173，179，180，183，??198，199，200，215，231，243，246，264，288，304，??314 | ??30 |
| ??7 | ??49.00 | ??86，91，117，119，120，128，153，160，161，177，??181，183，197，204，259，268，292 | ??30 |
| Sequence number | Time/min | Ion/amu | Residence time/ms |
| ??8 | ??51.80 | ??119，120，127，146，154，162，193，198，203，223，??250，264，265，267，279，285，286，289 | ??30 |
| ??9 | ??53.80 | ??121，125，146，160，162，184，188，195，198，206，??211，212，223，227，241，246，250，260，263，265，??267，269，277，285，287，306，354 | ??30 |
| ??10 | ??57.30 | ??66，162，172，207，222，226，238，241，260，263，??276，277，290，295，297，306，333，354 | ??30 |
| ??11 | ??58.88 | ??125，158，162，173，222，238，241，243，257，259，??272，278，279，295，297，299，314，316，327，332，??363 | ??30 |
| ??12 | ??60.52 | ??57，68，72，101，111，125，137，155，167，194，??195，196，198，208，225，236，239，241，243，250，??267，272，278，279，283，291，329，331，336，338 | ??30 |
| ??13 | ??62.27 | ??772，77，167，194，195，196，198，208，225，236，??239，248，250，252，254，267，269，281，283，323，??329，331，336，338 | ??30 |
| ??14 | ??65.10 | ??79，85，91，112，119，123，128，136，145，146，??168，212，213，240，246，255，267，269，274，283，??285，298，302，323，367，369，373，375，377 | ??30 |
| ??15 | ??67.64 | ??72，85，109，112，125，128，145，160，168，176，??220，236，241，258，262，271，286，302，304，311，??329，331，339，373，375，377 | ??30 |
| ??16 | ??70.81 | ??79，118，145，162，169，173，191，196，234，236，??238，246，258，260，263，288，290，303，309，316，??318，337，339 | ??30 |
| ??17 | ??72.83 | ??81，82，83，105，159，169，172，173，179，206， | ??30 |
| ??217，233，234，236，258，263，273，276，316，344，??429，449 |
| Sequence number | Time/min | Ion/amu | Residence time/ms |
| ??18 | ??73.99 | ??59，72，81，91，116，118，119，125，131，134，139，??189，191，206，233，238，241，247，252，263，273，??284，300，316，339，361，412，429，449 | ??30 |
| ??19 | ??76.25 | ??139，153，165，235，237，241，251，253，293，302，??308，330，339，384 | ??30 |
| ??20 | ??79.00 | ??98，116，119，131，148，161，173，201，222，235，??237，257，259，269，271，272，309，312，320，325，??340，352 | ??30 |
| ??21 | ??82.62 | ??116，125，131，173，222，238，250，253，255，256，??259，266，287，288，302，330，340，349，412，414 | ??30 |
| ??22 | ??86.00 | ??108，140，157，165，181，199，238，239，320，323，??340，341，343，376 | ??30 |
| ??23 | ??89.00 | ??77，88，97，116，120，135，140，141，160，163，??166，181，182，184，192，194，204，226，238，239，??288，318，320，333，341，343，349，354，356，376 | ??30 |
| ??24 | ??91.60 | ??93，139，141，165，181，183，197，221，223，229，??232，247，251，256，289，330，344，357，360，362，??373，449 | ??30 |
| ??25 | ??93.30 | ??59，72，100，108，121，147，165，179，180，183，??188，308，309，310，331，333，340，342，360，362，??364 | ??30 |
| ??26 | ??94.10 | ??59，72，100，121，163，165，179，180，184，186，??188，199，226，263，265，331，333，451 | ??30 |
| ??27 | ??96.50 | ??79，107，125，150，167，181，184，186，199，203，??218，250，252，253，265，267，308，318，323，344，??354，388，423，451 | ??30 |
4, the recovery of method (see Table 2 be attached to instructions last)
Embodiment:
In order to explain implementation method of the present invention more fully, provide the preparation embodiment of Fast Determination of Pesticide Residue in the garlic.These embodiments only are to explain rather than limit the scope of the invention.Wherein used raw material all has commercially available.
Embodiment 1
(1) garlic peeling, whole lobe claim 100g to use 500W microwave heating 90 seconds, and sample homogenization is handled;
(2) accurately take by weighing sample 10g and add 40mL acetonitrile and mL water, stir 2min with 20000 commentaries on classics/min homogenate; The 5mL acetonitrile is washed cutter head, and suction filtration, 15mL acetonitrile divide the cleaning residue three times, and is behind the interpolation water 1mL, to be clean;
(3) with 10mL acetonitrile and 10mL pure water difference pre-leaching C18 post (1000mg), above-mentioned filtrate is crossed the PSA column purification, use the 9mL acetonitrile, 3mL washes raffinate;
(4) eluent adds saturated 2mol/L phosphate buffer solution of 5mL salt and 6.5g salt, vibration 3min, static 15min;
(5) get upper solution, at 38 ℃ of following concentrating under reduced pressure; Concentrate is carried out the 2nd time purify,, use 30mL eluent B wash-out then, use 30mL eluent A wash-out again, collect eluent with eluent A5mL pre-leaching PSA post (500mg);
(6) add decane 50 μ L in the eluent, closely dried at 38 ℃ of following concentrating under reduced pressure, dry up with Nitrogen evaporator, 2mL constant volume liquid constant volume is collected in the sample flasket, measures for GC/MS.
Embodiment 2
(1) garlic peeling, whole lobe claim 200g to use 500W microwave heating 120 seconds, and sample homogenization is handled;
(2) accurately take by weighing sample 10.1g and add 60mL acetonitrile and 20mL water, stir 5min with 30000 commentaries on classics/min homogenate; The 5mL acetonitrile is washed cutter head, and suction filtration, 30mL acetonitrile divide the cleaning residue three times, and is behind the interpolation water 5mL, to be clean;
(3) with 20mL acetonitrile and 30mL pure water difference pre-leaching C18 post (1000mg), above-mentioned filtrate is crossed the PSA column purification, use the 15mL acetonitrile, 5mL washes raffinate;
(4) eluent adds saturated 2mol/L phosphate buffer solution of 5mL salt and 7g salt, vibration 3min, static 10min;
(5) get upper solution, at 38 ℃ of following concentrating under reduced pressure; Concentrate is carried out the 2nd time purify,, use 30mL eluent B wash-out then, use 30mL eluent A wash-out again, collect eluent with eluent A 5mL pre-leaching PSA post (500mg);
(6) add decane 50 μ L in the eluent, closely dried at 38 ℃ of following concentrating under reduced pressure, dry up with Nitrogen evaporator, 2mL constant volume liquid constant volume is collected in the sample flasket, measures for GC/MS.
Embodiment 3
(1) garlic peeling, whole lobe claim 150g to use 500W microwave heating 100 seconds, and sample homogenization is handled;
(2) accurately take by weighing sample 10g (being accurate to 0.1g) and add 50mL acetonitrile and 20mL water, stir 5min with 20000 commentaries on classics/min homogenate; The 5mL acetonitrile is washed cutter head, and suction filtration 30mL acetonitrile divides the cleaning residue three times, and is behind the interpolation water 5mL, to be clean;
(3) with 20mL acetonitrile and 30mL pure water difference pre-leaching C18 post (1000mg), above-mentioned filtrate is crossed the PSA column purification, use the 15mL acetonitrile, 5mL washes raffinate;
(4) eluent adds saturated 2mol/L phosphate buffer solution of 5mL salt and 8g salt, vibration 5min, static 10min;
(5) get upper solution, at 38 ℃ of following concentrating under reduced pressure; Concentrate is carried out the 2nd time purify,, use 30mL eluent B wash-out then, use 30mL eluent A wash-out again, collect eluent with eluent A 5mL pre-leaching PSA post (500mg);
(6) add decane 50 μ L in the eluent, closely dried at 38 ℃ of following concentrating under reduced pressure, dry up with Nitrogen evaporator, 2mL constant volume liquid constant volume is collected in the sample flasket, measures for GC/MS.
After the preferred embodiment that describes in detail, being familiar with this technology personage can be well understood to, can carry out various variations and modification not breaking away under above-mentioned claim and the spirit, all foundations technical spirit of the present invention is done any simple modification, equivalent variations and modification to above embodiment, all belongs to the scope of technical solution of the present invention.And the present invention also is not subjected to the restriction of the embodiment that gives an actual example in the instructions.
The recovery of table 2 method:
Claims (1)
1. the pre-treating method that pesticide multi-residues is measured in the garlic samples is characterized in that being undertaken by following step:
(1) garlic peeling, whole lobe claim 100-200g to use 500W microwave heating 90-120 second, and sample homogenization is handled;
(2) accurately take by weighing sample 10g ± 0.1, add 40-60mL acetonitrile and 10-20mL water, stir 2-5min with 20000-30000 commentaries on classics/min homogenate; The 5mL acetonitrile is washed cutter head, and suction filtration, 15-30mL acetonitrile divide the cleaning residue three times, and is behind the interpolation water 1-5mL, to be clean;
(3) with 10-20mL acetonitrile and 10-30mL pure water difference pre-leaching C18 post, above-mentioned filtrate is crossed the PSA column purification, use the 9-15mL acetonitrile, 3-5mL washes raffinate;
(4) eluent adds saturated 2mol/L phosphate buffer solution of 5mL salt and 6-10g salt, vibration 3-5min, static 10-15min;
(5) get upper solution, at 38 ℃ of following concentrating under reduced pressure; Concentrate is carried out the 2nd time purify,, use 30mL eluent B wash-out then, use 30mL eluent A wash-out again, collect eluent with eluent A5mL pre-leaching PSA post; Wherein eluent A is: acetone+normal hexane=50mL+50mL, eluent B are: acetone+normal hexane=20mL+80mL, employing eluent A constant volume liquid;
(6) add decane 50 μ L in the eluent, closely dried at 38 ℃ of following concentrating under reduced pressure, dry up with Nitrogen evaporator, adopt eluent A2mL constant volume liquid constant volume, be collected in the sample flasket, measure for GC/MS.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103105331A (en) * | 2013-01-22 | 2013-05-15 | 山东理工大学 | Sample processing method for detecting pesticide residue through biosensor |
| CN105158369A (en) * | 2015-09-06 | 2015-12-16 | 天津师范大学 | Establishment method of HPLC (High Performance Liquid Chromatography) fingerprint spectrum of allinase inactivated extract of six-peal red garlics |
| CN105181838A (en) * | 2015-09-06 | 2015-12-23 | 天津师范大学 | Method for establishing HPLC fingerprint of Liubanhong garlic enzymatic hydrolysis product |
| CN105628840A (en) * | 2015-12-28 | 2016-06-01 | 中国检验检疫科学研究院 | GC-Q-TOF/MS technology for detecting 708 kinds of pesticide residues in pome fruits |
| CN105651917A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | Detection technology for 708 kinds of pesticide residues GC-Q-TOF/MS in aquatic vegetables |
| CN105651916A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for 708 kinds of pesticide residues in melon fruit |
| CN107727771A (en) * | 2017-11-01 | 2018-02-23 | 广西沙田仙人滩农业投资有限公司 | The assay method of garlic residues of pesticides |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103105331A (en) * | 2013-01-22 | 2013-05-15 | 山东理工大学 | Sample processing method for detecting pesticide residue through biosensor |
| CN105158369A (en) * | 2015-09-06 | 2015-12-16 | 天津师范大学 | Establishment method of HPLC (High Performance Liquid Chromatography) fingerprint spectrum of allinase inactivated extract of six-peal red garlics |
| CN105181838A (en) * | 2015-09-06 | 2015-12-23 | 天津师范大学 | Method for establishing HPLC fingerprint of Liubanhong garlic enzymatic hydrolysis product |
| CN105181838B (en) * | 2015-09-06 | 2017-02-22 | 天津师范大学 | Method for establishing HPLC fingerprint of Liubanhong garlic enzymatic hydrolysis product |
| CN105628840A (en) * | 2015-12-28 | 2016-06-01 | 中国检验检疫科学研究院 | GC-Q-TOF/MS technology for detecting 708 kinds of pesticide residues in pome fruits |
| CN105651917A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | Detection technology for 708 kinds of pesticide residues GC-Q-TOF/MS in aquatic vegetables |
| CN105651916A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for 708 kinds of pesticide residues in melon fruit |
| CN107727771A (en) * | 2017-11-01 | 2018-02-23 | 广西沙田仙人滩农业投资有限公司 | The assay method of garlic residues of pesticides |
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Application publication date: 20100630 |