CN109212109A - The measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in a kind of tobacco and tobacco product - Google Patents
The measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in a kind of tobacco and tobacco product Download PDFInfo
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- CN109212109A CN109212109A CN201811429923.3A CN201811429923A CN109212109A CN 109212109 A CN109212109 A CN 109212109A CN 201811429923 A CN201811429923 A CN 201811429923A CN 109212109 A CN109212109 A CN 109212109A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in a kind of tobacco and tobacco product, it is characterized by: the iprodione in sample is all resolved into metabolin [iprodione takes off-(N- isopropyl formamide)] with alkaline solution, after hydrochloric acid acidification, with methylene chloride liquid-liquid extraction, filtering, nitrogen blow it is close dry after redissolved with acetonitrile, with the content of iprodione metabolin in liquid chromatography-mass spectrography measurement sample, thus in indirect determination sample iprodione total amount.Method of the invention overcomes the deficiency of prior art sample treatment, the blank of such substance-measuring is filled up, many references can be provided for the measurement of related residue limits and the exploitation of method and technology, sample-pretreating method and instrument testing conditions are optimized for tobacco sample, the method of the present invention has a following excellent results compared with prior art: the method for the present invention sample pretreatment process is simple, quickly, have the advantages that operation accurately, high sensitivity and reproducible.
Description
Technical field
The invention belongs to the remaining physical and chemical inspection technical fields of pesticide in tobacco product, and it is residual to relate generally to iprodione in tobacco
The determination techniques of allowance, specifically with alkaline solution by the iprodione in sample all resolve into metabolin [iprodione is de--
(N- isopropyl formamide)], after acidification, with methylene chloride liquid-liquid extraction, filtering, with different in liquid chromatography-mass spectrography measurement sample
The content of bacterium urea metabolin, thus in indirect determination sample iprodione content.
Background technique
Tobacco has become the important component in smoking safety issue as product, persticide residue problem is sucked,
Tobacco and tobacco product pesticide residue figureofmerit are important content of the various countries in the control of tobacco product quality, it has also become international city
An important factor for field tobacco leaf is evaluated and chosen and the important content that commodity inspection is carried out in tobacco international trade.Iprodione
(iprodione) also known as iprodione, belong to dicarboximide class, be a kind of broad spectrum activity contact killing type protective fungicide.This is killed
Microbial inoculum has an impact to each stage of development in the disease fungus history of life, is widely used in the disease control of fruit tree, vegetables, cereal
With the preservation and freshness of fruit.Be suitable for the vegetables such as foliar spray prevention and treatment graw mold of tomato, early blight and alternaria leaf spot of apple and
Fruit disease.Currently, China formulates MRL(maximum residue limit of the iprodione on tobacco, cucumber and tomato) value is respectively
0.1,2.0 and 5.0 mg/kg.The detection of iprodione residual quantity at present mostly uses GC-MS, HPLC, HPLC-MS method, pre-treatment
Method mainly has liquid-liquid extraction, Solid Phase Extraction, Dispersive solid phase extraction.These methods be using iprodione as test object,
But iprodione is easy to decompose in the sample, generate iprodione it is de--(N- isopropyl formamide) [Chinese agronomy notification, 2017,
33:150-153, Residue Degradation dynamic studies of the iprodione in Waxberry fruit], therefore only iprodione contains in test sample
Amount can accurately not assess the residual of iprodione in sample.Measuring method of the invention is based on this and proposes.
Summary of the invention:
The purpose of the present invention is intended to be directed to the statuses such as tobacco matrix situation is complicated, and sample type is more, overcomes prior art defect, mentions
It is combined with matrix with mark method for a kind of liquid-liquid extraction, directly with iprodione metabolism in liquid chromatography-mass spectrography measurement tobacco product
The measuring method of object residual quantity, thus in indirect determination sample iprodione content.This method quickly, can be detected accurately in tobacco
Iprodione remains total amount, and measurement result is accurate, measurement interference is few.
Mechanism of the invention is that the iprodione in sample is completely converted into iprodione in alkaline environment to take off-(N- isopropyl
Base formamide), by measurement iprodione it is de--the content indirect determination of (N- isopropyl formamide) sample in iprodione it is total
Amount, method is easy, provides new thinking for the iprodione determination of residual amount in tobacco.
The purpose of the present invention is achieved through the following technical solutions:
The measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in a kind of tobacco and tobacco product, with alkaline solution by sample
In iprodione all resolve into its metabolin i.e. iprodione it is de--(N- isopropyl formamide) use methylene chloride after hydrochloric acid acidification
Liquid-liquid extraction, filtering, nitrogen blow it is close dry after redissolved with acetonitrile, contained with iprodione metabolin in liquid chromatography-mass spectrography measurement sample
Amount, thus in indirect determination sample iprodione content.Specifically includes the following steps:
A, 1.0 g samples (being accurate to 0.01 g) extraction of sample: are accurately weighed in 50 mL tool lid centrifuge tube.It is added 0.2
Centrifuge tube, is then placed on vortex mixing shaker by 18 mL of sodium hydroxide solution of moL/L, with 2000 rpm rate oscillations
2 min.It is then placed into 30 min of water-bath in 90 DEG C of water-bath.It is cooled to room temperature, it is molten that the hydrochloric acid that mass fraction is 30% is added
2.0 mL of liquid mixes, 10 mL methylene chloride is added, with 2000 rpm rate oscillation, 2 min.Draw subnatant 1mL, nitrogen
It is redissolved after blowing close do with 1.0 mL acetonitriles, filters through 0.45 μm of organic phase filter membrane, detected with LC-MS；
B, prepared by standard working solution: weighing 10 mg(respectively and is accurate to 0.1 mg) iprodione metabolin standard items hold in 10 mL
In measuring bottle, selects acetonitrile to be dissolved and be settled to scale according to the solubility of standard items, be configured to primary standard stock solution.It moves
It takes 1.0 mL standard reserving solutions in 100 mL volumetric flasks, is settled to scale with acetonitrile, obtain secondary standard stock solution.Standard storage
Standby liquid is being protected from light, is saving at -18 DEG C.The secondary standard stock solution of different volumes is pipetted, and simultaneously with the dilution of blank sample extracting solution
Finally it is configured to the standard working solution with concentration gradient；
Specifically: pipetting secondary standard stock solution 25 μ L, 50 μ L, 100 μ L, 250 μ L, 500 μ L and 1000 μ L to 6 respectively
In a 10 mL volumetric flask, with blank sample extracting solution constant volume.
C, liquid chromatography-mass spectrography measures: drawing the standard working solution of the above prepared various concentration, injects liquid phase color
Spectrum-mass spectrograph；
D, the calculating of persticide residue measurement result
The quantitative analysis of residual quantity is carried out with external standard method, i.e., its respective concentration is carried out with the chromatographic peak area of iprodione metabolin
Regression analysis, obtains standard curve, and related coefficient is more than or equal to 0.99, is measured to the sample after extraction, measures object
Chromatographic peak area, substitute into standard curve, the residual quantity of the iprodione metabolin in sample is acquired, thus according to formulaThe content of iprodione in sample is calculated.
The liquid phase chromatogram condition of use are as follows: chromatographic column: Atlantis T3 (150 mm × 2.1mm, 3.0 μm)；Mobile phase
A: acetonitrile；Mobile phase B: 0.1% aqueous formic acid (volume fraction)；Isocratic elution, mobile phase A: Mobile phase B=4:1；Flow velocity:
0.2 mL/min；Column temperature: 40 DEG C；Sample volume: 10 μ L；The Mass Spectrometry Conditions of use: scanning mode: anion scanning;Electron spray
Ion source (ESI);Atomization gas flow is 60 psi;20 psi of gas curtain throughput;Auxiliary heating throughput is 60 psi;From
500 DEG C of sonization temperature;Residence time is 100 msec;5500 V of ionization voltage, the acquisition of Q1 scan pattern, sweep parameter are shown in Table
1。
Table 1 monitors ion and removes cluster voltage
| Chinese | Quota ion | Qualitative ion | Remove cluster voltage (V) |
| Iprodione metabolin | 243 | 159.9 | -80 |
Method of the invention overcomes the deficiency of prior art sample treatment, the characteristics of for iprodione and its metabolin,
Optimize sample-pretreating method and instrument testing conditions.The method of the present invention has following excellent results compared with prior art:
(1) it is decomposed since iprodione is easy in sample, generates iprodione and take off-(N- isopropyl formamide), therefore only detect sample
The content of iprodione can accurately not assess the residual condition of iprodione in sample in product.The present invention is in alkaline environment by sample
Iprodione in product is completely converted into iprodione and takes off-(N- isopropyl formamide), takes off-(N- isopropyl first by measurement iprodione
Amide) content indirect determination sample in iprodione total amount, experimental implementation is simple, quick, has filled up such substance-measuring
Blank.
(2) the method for the present invention has the advantages that operation accurate, high sensitivity and reproducible.
1. the detection of the method for the present invention limits:
The standard working solution of various concentration is injected into LC-MS, calculates detection limit (LOD), inspection with 3 times of signal-to-noise ratio (S/N=3)
Survey is limited to 0.08 mg/kg.
2. the repeatability and recovery of standard addition of the method for the present invention:
The standard solution of iprodione metabolin is added in the tobacco sample of blank, then carries out pre-treatment and LC-MS analysis,
And its rate of recovery is calculated according to scalar quantity and measured value, it the results are shown in Table 2.As can be seen from Table 2, the average of iprodione metabolin returns
Yield is 90.8%, and average relative standard's deviation (RSD) illustrates that the rate of recovery of the method for the present invention is high less than 5%, reproducible.
2 rate of recovery of table and repeatability (n=5)
Detailed description of the invention
Fig. 1 is measuring method flow chart of the invention (figure is as Figure of abstract).
The selection chromatography of ions figure of Fig. 2 mark-on sample of the present invention.
Specific embodiment
The present invention is described further below in conjunction with example, but is not the limitation present invention.
Example 1:
1. instrument and reagent:
Pesticide is standard items；Acetonitrile, formic acid are the residual grade of agriculture.
4000 quadrupole rod tandem mass spectrometer of API；Vortex oscillation instrument (Labnet company of the U.S.)；Sigma 3-30K centrifuge
(German Sigma company)；163 electronic balance of AE (sensibility reciprocal: 0.0001g) and 166 electronic balance of AE (sensibility reciprocal: 0.01g) (Switzerland
Mettler company).
2. sample treatment:
1.0 g samples (being accurate to 0.01 g) are accurately weighed in 50 mL tool lid centrifuge tube.The hydroxide of 0.2 moL/L is added
Then centrifuge tube is placed on vortex mixing shaker by 18 mL of sodium solution, with 2000 rpm rate oscillation, 2 min.Then it puts
It is placed in water-bath 30min in 90 DEG C of water-bath.It is cooled to room temperature, 2.0 mL of hydrochloric acid solution that mass fraction is 30% is added, mix
It is even, 10 mL methylene chloride are added, with 2000 rpm rate oscillation, 2 min.Draw subnatant 1mL, nitrogen blow it is close dry after use
1.0 mL acetonitriles redissolve, and filter through 0.45 μm of organic phase filter membrane, are detected with LC-MS；
3. preparing standard working solution: weighing 10 mg(respectively and be accurate to 0.1 mg) iprodione metabolin standard items hold in 10 mL
In measuring bottle, selects acetonitrile to be dissolved and be settled to scale according to the solubility of standard items, be configured to primary standard stock solution.It moves
It takes 1.0 mL standard reserving solutions in 100 mL volumetric flasks, is settled to scale with acetonitrile, obtain secondary standard stock solution.Standard storage
Standby liquid is being protected from light, is saving at -18 DEG C.Secondary standard stock solution 25 μ L, 50 μ L, 100 μ L, 250 μ L, 500 μ L are pipetted respectively
And 1000 in μ L to 6 10 mL volumetric flasks, with acetonitrile constant volume.
4. measuring method: the standard working solution of prepared various concentration being injected LC-MS, is carried out with external standard method residual
The quantitative analysis of allowance carries out regression analysis to its respective concentration with the chromatographic peak area of iprodione metabolin, obtains standard
Curve, related coefficient are more than or equal to 0.99.Sample after extraction is measured, the chromatographic peak face of iprodione metabolin is measured
Product substitutes into standard curve, acquires the residual quantity of iprodione metabolin in sample.Acquire the content of the iprodione metabolin in sample
Respectively 0.32 mg/kg, the content that iprodione is calculated is 0.43 mg/kg.
The liquid phase chromatogram condition of use are as follows: chromatographic column: Atlantis T3 (150 mm × 2.1mm, 3.0 μm)；Mobile phase
A:0.1% formic acid acetonitrile solution (volume fraction)；Mobile phase B: 0.1% aqueous formic acid (volume fraction)；Isocratic elution, flowing
Phase A: Mobile phase B=4:1；Flow velocity: 0.2 mL/min；Column temperature: 40 DEG C；Sample volume: 10 μ L；The Mass Spectrometry Conditions of use: scanning side
Formula: anion scanning;Electric spray ion source (ESI);Atomization gas flow is 60 psi;20 psi of gas curtain throughput;Auxiliary
Heating throughput is 60 psi;500 DEG C of ionization temperature;Residence time is 100 msec;Ionization voltage 5500 V, Q1
Scan pattern acquires
For the accuracy of judgment method, standard solution is added in this sample, so that the theory of iprodione metabolin contains in sample
Amount is 0.50 mg/kg, carries out sample pre-treatments ibid, the quota ion peak area of iprodione metabolin is measured with LC-MS,
Standard curve is substituted into, the content for acquiring iprodione metabolin in sample at this time is 0.48 mg/kg, TIANZHU XINGNAO Capsul 88.9%.
Example 2:
As described in Example 1, another tobacco sample is selected, iprodione metabolin is not detected in sample, and [iprodione takes off-(N- isopropyl
Base formamide)].
Claims (4)
1. the measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in a kind of tobacco and tobacco product, it is characterised in that: use alkali
Property solution by the iprodione in sample all resolve into its metabolin i.e. iprodione it is de--(N- isopropyl formamide), hydrochloric acid acidification
Afterwards, with methylene chloride liquid-liquid extraction, filtering, nitrogen blow it is close it is dry after redissolved with acetonitrile, with different bacterium in liquid chromatography-mass spectrography measurement sample
The content of urea metabolin, thus in indirect determination sample iprodione content.
2. the measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in tobacco according to claim 1 and tobacco product,
It is characterized by: specific step is as follows for the measuring method:
A, 1.0 g samples the extraction of sample: are accurately weighed in 50 mL tool lid centrifuge tube；The sodium hydroxide of 0.2 moL/L is added
Then centrifuge tube is placed on vortex mixing shaker by 18 mL of solution, with 2000 rpm rate oscillation, 2 min；Then it places
30 min of water-bath in 90 DEG C of water-bath；It is cooled to room temperature, 2.0 mL of hydrochloric acid solution that mass fraction is 30% is added, mix,
10 mL methylene chloride are added, with 2000 rpm rate oscillation, 2 min；Draw subnatant 1mL, nitrogen blow it is close dry after with 1.0
ML acetonitrile redissolves, and filters through 0.45 μm of organic phase filter membrane, is detected with LC-MS；
B, prepared by standard working solution: 10 mg iprodione metabolin standard items is weighed in 10 mL volumetric flasks, according to standard items
Solubility select acetonitrile dissolved and be settled to scale, be configured to primary standard stock solution；Pipette 1.0 mL standard inventories
Liquid is settled to scale with acetonitrile in 100 mL volumetric flasks, obtains secondary standard stock solution；Standard reserving solution be protected from light, -18 DEG C
Lower preservation；The secondary standard stock solution of different volumes is pipetted, and is diluted with blank sample extracting solution and is finally configured to have dense
Spend the standard working solution of gradient；
C, liquid chromatography-mass spectrography measures: drawing the standard working solution of the above prepared various concentration, injects liquid chromatogram-
Mass spectrograph；
D, the calculating of persticide residue measurement result
The quantitative analysis of residual quantity is carried out with external standard method, i.e., its respective concentration is carried out with the chromatographic peak area of iprodione metabolin
Regression analysis, obtains standard curve, and related coefficient is more than or equal to 0.99, is measured to the sample after extraction, measures object
Chromatographic peak area, substitute into standard curve, the residual quantity of the iprodione metabolin in sample is acquired, thus according to formulaThe content of iprodione is calculated.
3. the measuring method of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in tobacco according to claim 2 and tobacco product,
It is characterized by: the standard working solution manner of formulation with concentration gradient being finally configured in step b is as follows: pipetting respectively
In secondary standard stock solution 25 μ L, 50 μ L, 100 μ L, 250 μ L, 500 μ L and 1000 μ L to 6 10 mL volumetric flasks, use
Blank sample extracting solution constant volume.
4. the measurement side of the High Performance Liquid Chromatography/Mass Spectrometry of iprodione in tobacco according to claim 1 or 2 and tobacco product
Method, it is characterised in that: the liquid phase chromatogram condition of use are as follows: chromatographic column: Atlantis T3,150 mm of specification × 2.1mm, 3.0 μ
m；Mobile phase A: 0.1% formic acid acetonitrile solution；Mobile phase B: 0.1% aqueous formic acid；Isocratic elution, mobile phase A: Mobile phase B=
4:1；Flow velocity: 0.2 mL/min；Column temperature: 40 DEG C；Sample volume: 10 μ L；The Mass Spectrometry Conditions of use: scanning mode: anion is swept
It retouches;Electric spray ion source (ESI);Atomization gas flow is 60 psi;20 psi of gas curtain throughput;Auxiliary heats throughput
60 psi;500 DEG C of ionization temperature;Residence time is 100 msec;5500 V of ionization voltage, the acquisition of Q1 scan pattern.
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| CN112684034A (en) * | 2020-12-10 | 2021-04-20 | 中国烟草总公司郑州烟草研究院 | Non-target analysis method for detecting tobacco and tobacco products based on HPLC-QTOF MS technology |
| CN113295801A (en) * | 2021-06-04 | 2021-08-24 | 国家烟草质量监督检验中心 | Method for determining fluorosulfonyl in plant-derived food |
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