CN106290681A - The method for quick of Multi-pesticide residues and pre-treating method thereof in tomato sauce - Google Patents
The method for quick of Multi-pesticide residues and pre-treating method thereof in tomato sauce Download PDFInfo
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Abstract
The present invention relates to a kind of pre-treating method for Multi-pesticide residues in tomato sauce is used for quickly detecting, the method by extracting, purify, the step such as filtration forms.The invention still further relates to use this pre-treating method, use different instrument detection methods subsequently, it is achieved the method that Multi-pesticide residues in tomato sauce is used for quickly detecting.
Description
Technical field
The present invention relates to a kind of before in tomato sauce, Multi-pesticide residues is used for quickly detecting
Processing method, further relates to use this pre-treating method, use gas chromatogram-flame photometric detector,
Gas chromatography-electron capture detector and liquid chromatography-tandem level Four bar mass spectrum device are analyzed in tomato sauce
The method for quick of Multi-pesticide residues, belongs to field of detection of food safety.
Background technology
Can use Multiple Pesticides during tomato planting, these pesticidal properties are stable, the most degradable,
Can remain in during tomato processing in final products tomato sauce, form pesticide residues risk.
The pesticide of current domestic use, up to hundreds of kind, is likely to use hundreds of during tomato planting
Pesticide, how the Multiple Pesticides in tomato sauce is carried out across the quickly detection of kind be pesticide residues inspections
The difficult point surveyed.At present, in tomato sauce the detection method of many pesticide residues mainly include gas chromatography,
Liquid chromatography, gas chromatography-mass spectrography and LC/MS etc..Gas chromatography can detect
Organochlorine and pyrethroid, organophosphorus pesticide, liquid chromatography can detect carbamates
Pesticide, they broadly fall into the detection method of lower cost.Gas chromatography-mass spectrography and liquid chromatograph-
Mass spectrography detectable pesticide scope and kind are more, utilize multiple-reaction monitoring pattern (Multiple
Reaction Monitoring, MRM) in complex matrices, target pesticide can be realized high selectivity
Detection.These detection methods are required for agricultural product being carried out certain pre-treatment, to be suitable for
Carry out the sample of chromatography.
At present, the pre-treating method of tomato sauce Pesticide Residues detection is more, mainly includes that liquid liquid carries
Take, matrix solid phase extraction and dispersive solid-phase extraction etc..Wherein liquid-liquid extraction clean-up effect is poor, deposits
At bigger matrix interference and matrix effect；Matrix solid phase extraction processes to be needed sample is carried out craft
Grind, operate relative complex, it is impossible to realize high flux operation；And it is based on dispersive solid-phase extraction
QuEChERS method then utilizes certain adsorption stuffing simply to purify, simple to operate and quick,
Impurity interference is less.
On the other hand, existing pesticide residue detection method needs to carry out pin according to pesticide classification mostly
Sample pre-treatments to property, such as, China's standard GB/T/T 5009.218-2008 (fruit and
The mensuration of vegetable seed Multi-pesticide residues) in recorded use acetone, methanol, dichloromethane,
Sample is extracted by the multi-solvents such as benzene, normal hexane, ethanol.Existing pesticide variety then has number
Thousand kinds, different types of pesticide is also required to corresponding pre-treating method.Carry out sample targetedly respectively
Product pre-treatment will take considerable time and manpower and materials.Therefore, tomato sauce Pesticides how is realized residual
The quickly detection of allowance is the important topic of pesticide residue analysis detection field.Thus, at present for
Use unified pre-treating method, use different instruments according to the physicochemical properties of pesticide subsequently
Detection method realizes the quickly detection of Multiple Pesticides residual and there is actual demand.
Summary of the invention
It is an object of the invention to overcome existing pesticide residue detection method detection kind few, process
The shortcomings such as time length, Multiple Pesticides in a kind of low cost of exploitation, high coverage rate and efficient tomato sauce
The method that residual quantity carries out detecting；Meanwhile, the present invention is by using unified sample-pretreating method
Tomato sauce sample is extracted, purifies and concentrates, and uses different instrument detection sides later
Method, it is achieved Multiple Pesticides residual in tomato sauce is carried out quickly detection simply and easily.Institute of the present invention
State for pre-treating method that Multi-pesticide residues in tomato sauce is used for quickly detecting mainly by
Following steps form:
(1) in tomato sauce to be measured, add distilled water and optionally comprise the acetonitrile of 1% acetic acid, then
Add sodium chloride to saltout, use ultrasonic wave added to be dried with anhydrous magnesium sulfate after extracting, the highest
Speed is centrifugal, then removes supernatant；
(2) in this supernatant, add Graphon (GCB) and N-propyl group ethylenediamine bonding
Silica gel absorber (PSA) and anhydrous magnesium sulfate, centrifugal after vortex shaking, it is thus achieved that upper the most peace and quiet
Change liquid；
(3) the described supernatant scavenging solution obtained in step (2) is divided into three parts, uses nitrogen for first part
Gas is concentrated to dryness, then redissolves with normal hexane, then carries out membrane filtration, obtains dividing for GC-ECD
The liquid sample of analysis；Second part concentrates with nitrogen near dry, then redissolves with acetonitrile, carry out film mistake
Filter, obtains the liquid sample analyzed for GC-FPD；3rd part directly carries out membrane filtration,
Obtain the liquid sample analyzed for LC-MS/MS.
The present invention sample-pretreating method preferred embodiment in, step (1) meet such as
One or more in lower condition: the amount of taking of described tomato sauce to be measured is 5-10g, adding of distilled water
Entering amount is 5-10g, and the addition of sodium chloride is 1-10g, and the addition of acetonitrile is 5-40mL, anhydrous
The addition of magnesium sulfate is 5-10g；The ultrasound assisted extraction time is 30min；And/or described high speed
It is centrifuged and carries out 5min with 5000r/min.
In an embodiment of the sample-pretreating method of the present invention, step (2) meets as follows
One or more in condition: the mean diameter of described Graphon is 120-400mesh；Institute
The mean diameter of the silica gel absorber stating N-propyl group ethylenediamine bonding is 40-60mesh；And/or it is described
The usage amount scope of GCB and PSA is 50-250mg and 100-300mg respectively, is the most respectively
50mg and 250mg, and the usage amount of anhydrous magnesium sulfate be 0.5-2g, preferred 1g.
On the other hand, the invention provides one Multi-pesticide residues in tomato sauce is carried out soon
The method of speed detection, described method includes:
A () carries out processing tomato sauce to be measured with pre-treating method of the present invention, obtain three parts and treat
Survey fluid sample；
B () uses GC-ECD, GC-FPD and LC-MS/MS to obtain in step (a) respectively
To three parts of liquid sample be analyzed.
Method of the present invention compared with prior art has the advantage that
Owing to the present invention uses the pesticide residues in acetonitrile extraction tomato sauce, a certain amount of by adding
Sodium chloride, therefore (can include organophosphorus insecticide, organic chlorine agriculture chemicals, plan to common pesticide
Cinerins pesticide, carbamate chemicals for agriculture and other common pesticide) sufficiently extract,
Eliminate the chaff interference in tomato paste base, it is also possible to reduce instrument injection port and the damage of chromatographic column
Wound.
On the other hand, the present invention uses the mode of dispersive solid-phase extraction to purify sample extraction solution, logical
Cross and add the silica gel that a certain amount of GCB and N-propyl group ethylenediamine (PSA) is bonded, not only can have
Effect removes the chaff interferences such as the pigment in substrate and glucide, and cleanser be used in mixed way permissible
Obtain more preferable recovery of standard addition.
It addition, the pre-treating method of multiple types pesticide is unified by the present invention, i.e. use same
Plant sample-pretreating method and process Multiple Pesticides, the most complicated during saving Detecting Pesticide,
The most time-consumingly and most consume the step of solvent, enormously simplify and adopted for Multiple Pesticides residue detection in the past
With several samples pre-treatment time institute elapsed time, significantly reduce testing cost, utilize different inspections
Survey technology achieves Multiple Pesticides residue detection, the Pesticides Testing being very suitable in tomato sauce.
Accompanying drawing explanation
Fig. 1 is tomato sauce many Detection Technologies of Pesticide Residues schematic diagram of the present invention.
Fig. 2 is the recovery testu chromatogram of 32 kinds of organophosphorus pesticides.
In fig. 2, each chromatographic peak is respectively as follows: 1-Bayer 71628 according to label in figure；2-dichlorvos；
3-orthene；4-omethoate；5-demeton；6-phonamiphos；7-sulfotep；8-Azodrin；
9-thimet；10-Rogor；11-terbufos；12-Fonofos；13-isazofos；14-phosphamidon；
15-chlorpyrifos-methyl；16-parathion-methyl；17-fenifrothion；18-Malathion；19-chlopyrifos；
20-fenthion；21-parathion；22-isocarbophos；23-Isofenphos methyl；24-phosfolan；25-
Methidathion；26-fenamiphos；27-Profenofos；28-Ethodan；29-triazophos；30-phosmet；
31-Phosalone；32-coumafos.
Fig. 3 is the recovery testu chromatogram of 34 kinds of organochlorines and pyrethroid pesticide.
In figure 3, each chromatographic peak is respectively as follows: 1-Perchlorobenzene according to label in figure；2-α-Gamma Hexaochlorocyclohexane；
3-pentachloronitrobenzene；4-γ-Gamma Hexaochlorocyclohexane；5-β-Gamma Hexaochlorocyclohexane；6-heptachlor；7-δ-Gamma Hexaochlorocyclohexane；8-Bravo；
9-drinox；10-dicofol；11-Heptachlor epoxide B；12-Heptachlor epoxide A；13-procymidone；
14-o, p '-drip her；15-α-5a,6,9,9a-hexahydro-6,9-methano-2,4；16-p, p '-drip her；17-dieldrin；18-o, p '-dichloro-diphenyl-dichlorothane；
19-o, p '-clofenotane；20-p, p '-dichloro-diphenyl-dichlorothane；21-β-5a,6,9,9a-hexahydro-6,9-methano-2,4；22-p, p '-clofenotane；23-biphenyl chrysanthemum
Ester；24-5a,6,9,9a-hexahydro-6,9-methano-2,4 sulfuric ester；25-Fenpropathrin；26-gamma cyhalothrin；27-mirex；28/29-
Permethrin；30-pyridaben；31/35/36-taufluvalinate；32/33/34-cypermethrin；37/38-
Esfenvalerate；39/40-decis；41-Difenoconazole.
Fig. 4 A-4C figure is the liquid chromatography-tandem level Four bar mass spectrum MRM of 19 kinds of other common pesticide
The recovery testu chromatogram obtained.
Fig. 5 shows the experimental result that organophosphorus insecticide recovery of standard addition is tested.
Fig. 6 shows the experimental result of organophosphorus insecticide repeated experiment.
Fig. 7 shows organochlorine and the experimental result of pyrethroid pesticide recovery of standard addition experiment.
Fig. 8 shows organochlorine and the experimental result of pyrethroid pesticide repeated experiment.
Detailed description of the invention
As it is shown in figure 1, the present invention uses unified sample-pretreating method, tomato sauce sample is carried out
After extracting, purifying and concentrate, then by different instrument detection methods, it is achieved in tomato sauce
The quick detection of Multiple Pesticides residual.
Before this invention in processing method, the acetonitrile added in step (1) optionally comprises 1%
Acetic acid, the alkali unstability pesticide in sample can be carried out stable by the addition of acetic acid further, thus
Improve Detection accuracy.
In step (3), obtain when the liquid sample that GC-FPD analyzes, to sample
Carry out nitrogen and blow near dry.Described " the most dry " refers to be dried up completely by sample, but in the sample
Substantially blow without i.e. stopping nitrogen in the presence of visible liquid solvent, after slightly placing, acetonitrile can be added further
Redissolve.Specifically, " the most dry " may refer to the acetonitrile solvent content in sample at below 5wt%.
GCB and PSA used in all specific embodiments of the present invention, refer to Graphon and
The silica gel adsorption filler of N-propyl group ethylenediamine bonding, its specifying information is as follows:
Name of product: GCB, mean diameter: 120-400mesh；Name of product: PSA, averagely
Particle diameter: 40-60mesh, (being purchased from Tianjin Beaune Ai Jieer company).
Concrete sample pretreatment process employed in each embodiment of the present invention is as follows:
(1) sample preparation: weigh about 500g tomato sauce, standby after being sufficiently stirred for；
(2) extract: weigh in the 50mL plastic centrifuge tube of 5g sample (accurately to 0.01g),
Add 5mL ultra-pure water, make water and tomato sauce fully mix；The most accurately add 20mL containing 1% second
The acetonitrile of acid and 3g sodium chloride, vibrate 2min with turbula shaker；Put into ultrasound wave afterwards to occur
Device, ultrasound assisted extraction 30min, wherein supersonic generator is built with ice bag, prevents ultrasonic
During extraction, temperature rises；Add 5g anhydrous magnesium sulfate, acutely shake, allow anhydrous magnesium sulfate
Moisture in adsorption sample as far as possible；It is centrifuged 5min again, it is thus achieved that the supernatant after Li Xin with 5000r/min
Extract solution.
(3) purify: weigh mixing cleanser 1.3g in advance (by 50mg GCB, 250mg PSA
Form with 1g anhydrous magnesium sulfate) in 50mL centrifuge tube, add upper strata extracting solution 15mL；Will
Centrifuge tube vibrates 3min on turbula shaker, it is ensured that extracting solution and cleanser are sufficiently mixed；Afterwards
It is centrifuged 5min with 5000r/min.
(4) concentrate and redissolve: the supernatant scavenging solution obtained in step (3) is divided into three parts, point
Do not carry out lower column processing:
Take 4mL supernatant scavenging solution nitrogen to be concentrated to dryness, then redissolve with normal hexane, then carry out film
Filter, obtain the liquid sample analyzed for GC-ECD；
Take 4mL supernatant scavenging solution, concentrate with nitrogen near dry, then redissolve with acetonitrile, carry out membrane filtration,
Obtain the liquid sample analyzed for GC-FPD；
Take the supernatant scavenging solution of appropriate volume, carry out membrane filtration, obtain analyzing for LC-MS/MS
Liquid sample.
On the other hand, the invention still further relates to, respectively by different detection meanss, use above-mentioned front place
The liquid sample that reason method obtains is used for quickly detecting.
Detection technique of the present invention is for using gas chromatogram-flame photometric detector
(GC-FPD), gas chromatography-electron capture detector (GC-ECD) and liquid chromatography-tandem four
Level bar mass spectrography (LC-MS/MS) is as instrument detection method.The detecting instrument particular type used
Number it is, and uses following operating parameter:
(1) organochlorine, pyrethroid pesticide (GC-ECD detection): chromatographic column: DB-35ms
(30m×0.25mm×0.25μm)；Temperature programming: 100 DEG C keep 2min, then with 10 DEG C
/ min is warming up to 300 DEG C, keeps 18min；Carrier gas: high pure nitrogen, constant current mode, flow velocity is
1.0mL/min；Injector temperature: 220 DEG C；Input mode: split sampling, split ratio: 10:1；
Sample size: 1 μ L；Detector temperature 320 DEG C.
(2) organophosphorus pesticide (GC-FPD detection): chromatographic column: DB-5ms (30m × 0.25
mm×0.25μm)；Temperature programming: 80 DEG C keep 1min, are then warming up to 10 DEG C/min
280 DEG C, keep 5min, be warming up to 300 DEG C with 20 DEG C/min, keep 18min；Carrier gas:
High pure nitrogen, constant current mode, flow velocity is 1.0mL/min；Injector temperature: 220 DEG C；Sample introduction
Mode: Splitless injecting samples；Sample size: 1 μ L；Detector temperature 250 DEG C；H2 flow: 75
ML/min, air mass flow: 100mL/min.
(3) other common pesticide (LC-MS/MS detection): Ultra Performance Liquid Chromatography condition chromatography
Post Waters ACQUITY UPLC CSH C18 post (2.1mm × 100mm.i d., 1.7 μm)；
Column temperature 40 DEG C；Sample temperature 20 DEG C；Sampling volume 2 μ L.Mobile phase A is containing 0.1% (body
Fraction) formic acid-aqueous solution, Mobile phase B is containing 0.1% (volume fraction) formic acid-acetonitrile, ladder
Degree elution program is shown in Table 1.Flow velocity is 0.2mL/min.
Table 1:UPLC eluent gradient condition
Mass Spectrometry Conditions: use electric spray ion source, ESI holotype；Capillary voltage: 3.0kV；
Electron spray ionisation ((ESI) source temperature: 150 DEG C；Desolventizing temperature: 500 DEG C；Desolventizing gas
Flow ((nitrogen): 1000L/h；Taper hole air-flow: 150L/h；Collision gas argon: 0.15mL/min；
Photomultiplier voltage: 535V；Scan mode: multiple-reaction monitoring pattern (MRM).
Other common pesticide of table 2:19 kind mass spectrometry parameters that UPLC-MS/MS analyzes under MRM pattern
Different types of pesticide is added, through sample pre-treatments and the inspection of present invention proposition in tomato sauce
Survey technology route, obtains mark-on in conjunction with GC-ECD, GC-FPD and LC-MS/MS detection and reclaims
The chromatogram of experiment, as in Figure 2-4.
The technology path that the present invention provides is equal to recovery of standard addition, the repeated experiment of multiple types pesticide
Meet the agriculture of regulation in GB/T 27404-2008 " Good Laboratory controls specification food Physico-chemical tests "
Medicine residue detection requirement, sees Fig. 5-Fig. 8 and the record of table 3 below-table 5.
The average recovery of standard addition of table 3:32 kind organophosphorus insecticide and relative standard deviation
Table 4:34 kind organochlorine and the average recovery of standard addition of pyrethroid pesticide and relative standard deviation
The average recovery of standard addition of table other common pesticide of 5:19 kind and relative standard deviation
From the data in above table and the data in accompanying drawing, the quickly side of detection of the present invention
Method is by using same pre-treating method and using different detection method to detect subsequently, it is achieved
Multi-pesticide residues detection fast and accurately, it is thus achieved that excellent result.
The method of the present invention is compared with the prior art
The sample-pretreating method step that the present invention provides includes supersound extraction, saltouts, centrifugal, only
Changing and concentrate, single sample elapsed time is about 1 hour；And according to industry standard NYT 761-2008
The content that text provides, this standard needs that organochlorine and pyrethroid pesticide are detected project and enters
The SPE of row sample purifies, and elapsed time is about single sample 2 hours, organophosphorus insecticide simultaneously
Detection project does not purify, but is directly entered gas chromatographic detection, and instrument and chromatograph are caused one
Fixed damage.Concrete contrast sees the record of table 6 below.
Table 6: the present invention and the contrast of NYT 761-2008
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, but, the present invention is also
It is not limited to the detail in above-mentioned embodiment, in the technology concept of the present invention, permissible
Technical scheme is carried out multiple simple variant, and these simple variant belong to the present invention's
Protection domain.
Claims (5)
1. one kind is used for the pre-treatment side being used for quickly detecting Multi-pesticide residues in tomato sauce
Method, described pre-treating method comprises the steps of:
(1) in tomato sauce to be measured, add distilled water and optionally comprise the acetonitrile of 1% acetic acid, then
Add sodium chloride to saltout, use ultrasonic wave added to be dried with anhydrous magnesium sulfate after extracting, the highest
Speed is centrifugal, then removes supernatant；
(2) the described supernatant obtained in step (1) adds Graphon and N-propyl group
The silica gel absorber of ethylenediamine bonding and anhydrous magnesium sulfate, centrifugal after vortex shaking, it is thus achieved that supernatant
Scavenging solution；
(3) the described supernatant scavenging solution obtained in step (2) is divided into three parts, first part of use
Nitrogen is concentrated to dryness, then redissolves with normal hexane, then carries out membrane filtration, obtains for GC-ECD
The liquid sample analyzed；Second part concentrates with nitrogen near dry, then redissolves with acetonitrile, carry out film
Filter, obtain the liquid sample analyzed for GC-FPD；3rd part directly carries out membrane filtration,
Obtain the liquid sample analyzed for LC-MS/MS.
2. pre-treating method as claimed in claim 1, wherein, described step (1) meets such as
One or more in lower condition:
The amount of taking of described tomato sauce to be measured is 5-10g, and the addition of distilled water is 5-10g, chlorination
The addition of sodium is 1-10g, and the addition of acetonitrile is 5-40mL, and the addition of anhydrous magnesium sulfate is
5-10g；
The ultrasound assisted extraction time is 30min；And/or
Described high speed centrifugation carries out 5min with 5000r/min.
3. pre-treating method as claimed in claim 2, wherein, described step (2) meets such as
One or more in lower condition:
The mean diameter of described Graphon is 120-400mesh；
The mean diameter of the silica gel absorber of described N-propyl group ethylenediamine bonding is 40-60mesh；With/
Or
The usage amount model of the silica gel absorber of described Graphon and described N-propyl group ethylenediamine bonding
Enclosing is 50-250mg and 100-300mg respectively, and the usage amount of anhydrous magnesium sulfate is 0.5-2g.
4. pre-treating method as claimed in claim 3, wherein, in described step (2), institute
The usage amount of the silica gel absorber stating Graphon and described N-propyl group ethylenediamine bonding is respectively
In 50mg and 250mg, and described step (2), the usage amount of anhydrous magnesium sulfate is 1g.
5. method Multi-pesticide residues in tomato sauce being used for quickly detecting, described method
Comprise the following steps:
A () uses the pre-treating method according to any one of claim 1-4 to enter described tomato sauce
Row processes, and obtains three parts of liquid sample；
B () uses GC-ECD, GC-FPD and LC-MS/MS to obtain in step (a) respectively
To three parts of liquid sample be analyzed.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108226343A (en) * | 2018-01-08 | 2018-06-29 | 中国检验检疫科学研究院综合检测中心 | Multiple Pesticides method for detecting residue in a kind of vegetables and fruits |
| CN108663446A (en) * | 2018-05-08 | 2018-10-16 | 江苏安舜技术服务有限公司 | A kind of assay method that spirulina middle peasant is residual |
| CN108693003A (en) * | 2018-04-26 | 2018-10-23 | 许昌学院 | A kind of method of leafy vegetable Detecting Pesticide sample pre-treatments |
| CN109142592A (en) * | 2018-11-09 | 2019-01-04 | 中华人民共和国桂林海关 | A kind of method of pyridaben residual quantity in measurement Siraitia grosvenorii |
| CN109668885A (en) * | 2019-02-27 | 2019-04-23 | 无锡中德伯尔生物技术有限公司 | The detection method of procymidone in a kind of vegetables |
| CN110057940A (en) * | 2019-05-14 | 2019-07-26 | 黑龙江八一农垦大学 | The detection method of Quizalofop-p-Ethyl Residues amount in a kind of rde bean |
| CN110057928A (en) * | 2019-02-27 | 2019-07-26 | 中国热带农业科学院农产品加工研究所 | A kind of ultra performance liquid chromatography tandem mass spectrometry detecting captan residual quantity in tomato |
| CN110954525A (en) * | 2019-09-23 | 2020-04-03 | 上海如海光电科技有限公司 | Raman rapid detection method for sibutramine in weight-reducing tea |
| CN112098553A (en) * | 2020-09-11 | 2020-12-18 | 安徽中创食品检测有限公司 | Method for detecting capsaicin compounds in duck neck |
| CN113884606A (en) * | 2021-10-22 | 2022-01-04 | 生态环境部南京环境科学研究所 | Method for determining 47 pesticide residues in honey and bee pollen |
| CN118443853A (en) * | 2024-07-04 | 2024-08-06 | 甘肃药业集团科技创新研究院有限公司 | Pretreatment solid-phase extraction column for detecting pesticide residues in hawthorns, filling method and using method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776656A (en) * | 2010-01-15 | 2010-07-14 | 新疆出入境检验检疫局检验检疫技术中心 | Method for measuring patulin in fruit jam and vegetable paste |
| CN102393425A (en) * | 2011-10-20 | 2012-03-28 | 新疆出入境检验检疫局检验检疫技术中心 | Method for detecting residual amount of streptomycin and dihydrostreptomycin in tomato sauce |
-
2015
- 2015-06-12 CN CN201510324698.7A patent/CN106290681A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776656A (en) * | 2010-01-15 | 2010-07-14 | 新疆出入境检验检疫局检验检疫技术中心 | Method for measuring patulin in fruit jam and vegetable paste |
| CN102393425A (en) * | 2011-10-20 | 2012-03-28 | 新疆出入境检验检疫局检验检疫技术中心 | Method for detecting residual amount of streptomycin and dihydrostreptomycin in tomato sauce |
Non-Patent Citations (4)
| Title |
|---|
| 李锋格 等: "出口番茄酱中30种有机磷农药残留量分析方法的研究", 《中国卫生检验杂志》 * |
| 李锋格 等: "气相色谱-质谱法同时测定番茄制品中拟除虫菊酯类农药残留", 《分析化学》 * |
| 粟有志 等: "QuEChERS－液相色谱／串联质谱法测定果蔬及其制品中矮壮素和缩节胺残留", 《分析科学学报》 * |
| 陈士恒 等: "QuEChERS-超高效液相色谱-串联四级杆质谱法快速检测番茄酱中19种常见农药残留量", 《食品安全质量检测学报》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN108693003A (en) * | 2018-04-26 | 2018-10-23 | 许昌学院 | A kind of method of leafy vegetable Detecting Pesticide sample pre-treatments |
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