CN105699536A - Detection method for thiophanate-methyl residual amount in apples - Google Patents
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to the field of food safety inspection and discloses a detection method for thiophanate-methyl residual amount in apples. The detection method comprises the following steps: preparing a standard stock solution; preparing a standard working solution; preparing a sample; extracting the sample; eluting the sample; secondarily concentrating and filtering; performing chromatography determination; performing mass spectrum determination; and performing instrument determination and quantitative analysis. According to the detection method provided by the invention, a liquid chromatograph/mass spectrometer is used for detecting the thiophanate-methyl residual amount in apples, the detection result is accurate, the operation is simple, convenient and quick, and the detection demand on the thiophanate-methyl residual amount in apples in the market can be met.
Description
Technical field
The present invention relates to field of detection of food safety, specifically the detection method of thiophanate-methyl residual quantity in a kind of Fructus Mali pumilae。
Background technology
Fructus Mali pumilae is one of modal fruit。Apple aroma is sweet, and mouthfeel is sharp and clear, and rich in abundant nutrition, is the hat of the big fruit in the world four。The nature and flavor of Fructus Mali pumilae are gentle, containing abundant carbohydrate, vitamin and trace element, there are saccharide, organic acid, pectin, protein, calcium, phosphorus, potassium, ferrum, vitamin A, vitamin B, vitamin C and dietary fiber, another containing malic acid, tartaric acid, carotene, is that all vegetables and fruits Middle nutrition are worth closest to perfect one。
In order to make Fructus Mali pumilae prevent fungus disease in the storage phase, it is necessary to Fructus Mali pumilae is carried out Preservation Treatment。Although having research and the report of the apple fresh-keeping new techniques such as film, reduced pressure treatment, HIGH PRESSURE TREATMENT, crude antistaling agent, bio-preservative at present, but being subject to the impact of the factor such as technology, cost, China is still chemical preservation antistaling agent for what the process of Fructus Mali pumilae anti-corrosive fresh-keeping commonly used。Fructus Mali pumilae is when carrying out fresh-keeping, and the most frequently used chemical preservation antistaling agent is thiophanate-methyl, has another name called thiophanate methyl, is inhale low toxicity antibacterial in a kind of broad spectrum activity, has interior suction, preventive and therapeutic action。At present, for the determination method of thiophanate-methyl, that has reported mainly has high performance liquid chromatography, gas chromatogram and euzymelinked immunosorbent assay (ELISA) etc.。Gas chromatography or liquid chromatography are subject to impurity interference, and sensitivity is low；Enzyme-linked immunoassay method operating process is loaded down with trivial details, and condition requires harshness。
Summary of the invention
It is an object of the invention to provide the detection method of thiophanate-methyl residual quantity in a kind of Fructus Mali pumilae, with the problem solving to propose in above-mentioned background technology。
For achieving the above object, the present invention provides following technical scheme:
The detection method of thiophanate-methyl residual quantity in a kind of Fructus Mali pumilae, step is as follows:
1) preparation of standard reserving solution, accurately weigh thiophanate-methyl standard substance 10mg with 100,000/balance in beaker, be accurate to 0.1mg, add acetonitrile and dissolve and be settled in 10mL volumetric flask, it is configured to the list mark storing solution that concentration is 1000 μ g/mL, 1 DEG C～4 DEG C preservations in refrigerator；
2) preparation of standard working solution, accurately pipette 1mL mono-mark storing solution and be placed in the brown volumetric flask of 100mL, it is settled to scale with acetonitrile, it is made into the standard intermediate liquid of 10 μ g/mL, pipette appropriate standard intermediate liquid as required, be diluted to the standard working solution of 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL with acetonitrile-aqueous solution, various standard solution seal and are stored in 1 DEG C～4 DEG C refrigerators；
3) prepared by sample, takes 1000g belt leather Fructus Mali pumilae sample and chooses a certain amount of sample, size-reduced or tissue mashing machine's homogenate, it is thus achieved that testing sample through quartering, loads in sample sack, and in sealing, labelling, 1 DEG C～4 DEG C refrigerators, cold preservation is stand-by；
4) sample extraction, takes testing sample, adds the ether of 5～8 times amount, supersound extraction 8～10min again after vortex oscillation 2～3min, adds 2～4g sodium chloride, is vortexed again for 4～5min, and 5500～6000r/min is centrifuged 10～12min；Divide 2 times again and add 8～10 times amount ether, the centrifugal 12～15min of 5500～6000r/min after vortex oscillation 6～7min, merge organic facies, and adopt Parallel evaporator to carry out first time concentration, it is thus achieved that once concentration liquid；
5) sample elution, activated carbon pillar is first activated with eluent, uses elution after then once concentration liquid is poured into activated carbon pillar, it is thus achieved that eluting collects liquid, described eluent is the equal-volume mixed liquor of ethyl acetate and acetone, and consumption is 10～12 times that once concentration liquid is long-pending；
6) secondary concentration and filtration, collects eluting liquid and adopts the mode that nitrogen blows promotion eluent volatilization to carry out second time concentration, it is thus achieved that secondary concentration liquid, secondary concentration liquid adopts methanol constant volume to 2ml, adopting 0.30 μm of membrane filtration, it is thus achieved that filtrate, filtrate feed flow matter combined instrument measures；
7) chromatographic determination；
8) mass spectroscopy；
9) Instrument measuring, the program of sample feeding is: reagent blank, standard working curve, sample blank, sample add and actual sample, repeats above step；
10) quantitative approach, by step 9) sample introduction, with chromatographic work station Criterion working curve, sample adopts working curve quantitative。
As the present invention further scheme: step 2) in, acetonitrile-aqueous solution is containing 0.15% formic acid, and in acetonitrile-aqueous solution, acetonitrile is 1:1 with the volume ratio of water。
As the present invention further scheme: step 8) in, the quota ion of thiophanate-methyl is to for 343,113/151,074, and qualitative ion pair is 343,131/118,123, S-lens voltages is 76V, and collision voltage is 18；51, scan pattern is positive, and retention time is 7.6min, and ion source is electric spray ion source, scan mode is positive and negative switched scan, detection mode is multiple-reaction monitoring, and capillary temperature is 350 DEG C, and evaporating temperature is 300 DEG C, electron spray voltage is+3500 (-3000) V, sheath gas is 30arb, and assisted gas is 10arb, and collision gas is argon。
As the present invention further scheme: step 7) in, chromatographic column is HypersilGOLDC18, and thickness is 1.9 μm, and internal diameter is 2.1mm × 50mm, and column temperature is 35 DEG C, and sample size is 2 μ L, adopts gradient elution。
As the present invention further scheme: step 7) in condition of gradient elution as follows
| Time (min) | Flow velocity (ml/min) | Acetonitrile (%) | Water (%) containing 0.15% formic acid |
| 0.00 | 0.2 | 10.0 | 90.0 |
| 2.00 | 0.2 | 10.0 | 90.0 |
| 11.00 | 0.2 | 95.0 | 5.0 |
| 14.00 | 0.2 | 95.0 | 5.0 |
| 14.10 | 0.2 | 10.0 | 90.0 |
| 18.00 | 0.2 | 10.0 | 90.0 |
。
Compared with prior art, the invention has the beneficial effects as follows: the present invention carries out the detection of thiophanate-methyl residual quantity in Fructus Mali pumilae by LC-MS instrument, testing result is accurate, easy and simple to handle, quick, it is possible to meet on market to the testing requirement of thiophanate-methyl residual quantity in Fructus Mali pumilae。
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in more detail。
Embodiment 1
The detection method of thiophanate-methyl residual quantity in a kind of Fructus Mali pumilae, step is as follows:
1) preparation of standard reserving solution, accurately weigh thiophanate-methyl standard substance 10mg with 100,000/balance in beaker, be accurate to 0.1mg, add acetonitrile and dissolve and be settled in 10mL volumetric flask, it is configured to the list mark storing solution that concentration is 1000 μ g/mL, 4 DEG C of preservations in refrigerator；
2) preparation of standard working solution, accurately pipette 1mL mono-mark storing solution and be placed in the brown volumetric flask of 100mL, it is settled to scale with acetonitrile, it is made into the standard intermediate liquid of 10 μ g/mL, pipette appropriate standard intermediate liquid as required, the standard working solution of 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL it is diluted to acetonitrile-aqueous solution, wherein acetonitrile-aqueous solution is containing 0.15% formic acid, in acetonitrile-aqueous solution, acetonitrile is 1:1 with the volume ratio of water, and various standard solution seal and are stored in 4 DEG C of refrigerators；
3) prepared by sample, takes 1000g belt leather Fructus Mali pumilae sample and chooses a certain amount of sample, size-reduced or tissue mashing machine's homogenate, it is thus achieved that testing sample through quartering, loads in sample sack, and in sealing, labelling, 4 DEG C of refrigerators, cold preservation is stand-by；
4) sample extraction, takes testing sample 2g, adds the ether of 5 times amount, supersound extraction 8min again after vortex oscillation 2min, adds 2g sodium chloride, is vortexed again for the centrifugal 10min of 4min, 5500r/min；Divide 2 times again and add 8 times amount ether, the centrifugal 12min of 5500r/min after vortex oscillation 6min, merge organic facies, and adopt Parallel evaporator to carry out first time concentration, it is thus achieved that once concentration liquid；
5) sample elution, activated carbon pillar is first activated with eluent, uses elution after then once concentration liquid is poured into activated carbon pillar, it is thus achieved that eluting collects liquid, described eluent is the equal-volume mixed liquor of ethyl acetate and acetone, and consumption is 10 times that once concentration liquid is long-pending；
6) secondary concentration and filtration, collects eluting liquid and adopts the mode that nitrogen blows promotion eluent volatilization to carry out second time concentration, it is thus achieved that secondary concentration liquid, secondary concentration liquid adopts methanol constant volume to 2ml, adopting 0.30 μm of membrane filtration, it is thus achieved that filtrate, filtrate feed flow matter combined instrument measures；
7) chromatographic determination, chromatographic column is HypersilGOLDC18,1.9 μm, 2.1mm × 50mm, and column temperature is 35 DEG C, and sample size is 2 μ L, adopts gradient elution, and condition of gradient elution is as follows:
8) mass spectroscopy, antistaling agent standard solution is respectively adopted flow injection direct injected, compound parent ion is determined by full scan, again parent ion is carried out second order ms scanning, obtain fragment ion, by optimizing S-Lens, the parameters such as collision energy are optimized, obtain second order ms figure, obtain quota ion pair, qualitative ion pair, S-lens voltage, collision voltage, scan pattern and retention time, the quota ion of thiophanate-methyl is to for 343, 113/151, 074, qualitative ion pair is 343, 131/118, 123, S-lens voltage is 76V, collision voltage is 18；51, scan pattern is positive, and retention time is 7.6min, and ion source is electric spray ion source, scan mode is positive and negative switched scan, detection mode is multiple-reaction monitoring, and capillary temperature is 350 DEG C, and evaporating temperature is 300 DEG C, electron spray voltage is+3500 (-3000) V, sheath gas is 30arb, and assisted gas is 10arb, and collision gas is argon；
9) Instrument measuring, the program of sample feeding is: reagent blank, standard working curve, sample blank, sample add and actual sample, repeats above step；
10) quantitative approach, by step 9) sample introduction, with chromatographic work station Criterion working curve, sample adopts working curve quantitative。
Embodiment 2
The detection method of thiophanate-methyl residual quantity in a kind of Fructus Mali pumilae, step is as follows:
1) preparation of standard reserving solution, accurately weigh thiophanate-methyl standard substance 10mg with 100,000/balance in beaker, be accurate to 0.1mg, add acetonitrile and dissolve and be settled in 10mL volumetric flask, it is configured to the list mark storing solution that concentration is 1000 μ g/mL, 2 DEG C of preservations in refrigerator；
2) preparation of standard working solution, accurately pipette 1mL mono-mark storing solution and be placed in the brown volumetric flask of 100mL, it is settled to scale with acetonitrile, it is made into the standard intermediate liquid of 10 μ g/mL, pipette appropriate standard intermediate liquid as required, the standard working solution of 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL it is diluted to acetonitrile-aqueous solution, wherein acetonitrile-aqueous solution is containing 0.15% formic acid, in acetonitrile-aqueous solution, acetonitrile is 1:1 with the volume ratio of water, and various standard solution seal and are stored in 2 DEG C of refrigerators；
3) prepared by sample, takes 1000g belt leather Fructus Mali pumilae sample and chooses a certain amount of sample, size-reduced or tissue mashing machine's homogenate, it is thus achieved that testing sample through quartering, loads in sample sack, and in sealing, labelling, 2 DEG C of refrigerators, cold preservation is stand-by；
4) sample extraction, takes testing sample 1.5g, adds the ether of 8 times amount, supersound extraction 10min again after vortex oscillation 3min, adds 4g sodium chloride, is vortexed again for the centrifugal 12min of 5min, 6000r/min；Divide 2 times again and add 10 times amount ether, the centrifugal 15min of 6000r/min after vortex oscillation 7min, merge organic facies, and adopt Parallel evaporator to carry out first time concentration, it is thus achieved that once concentration liquid；
5) sample elution, activated carbon pillar is first activated with eluent, uses elution after then once concentration liquid is poured into activated carbon pillar, it is thus achieved that eluting collects liquid, described eluent is the equal-volume mixed liquor of ethyl acetate and acetone, and consumption is 12 times that once concentration liquid is long-pending；
6) secondary concentration and filtration, collects eluting liquid and adopts the mode that nitrogen blows promotion eluent volatilization to carry out second time concentration, it is thus achieved that secondary concentration liquid, secondary concentration liquid adopts methanol constant volume to 2ml, adopting 0.30 μm of membrane filtration, it is thus achieved that filtrate, filtrate feed flow matter combined instrument measures；
7) chromatographic determination, chromatographic column is HypersilGOLDC18,1.9 μm, 2.1mm × 50mm, and column temperature is 35 DEG C, and sample size is 2 μ L, adopts gradient elution, and condition of gradient elution is as follows:
| Time (min) | Flow velocity (ml/min) | Acetonitrile (%) | Water (%) containing 0.15% formic acid |
| 0.00 | 0.2 | 10.0 | 90.0 |
| 2.00 | 0.2 | 10.0 | 90.0 |
| 11.00 | 0.2 | 95.0 | 5.0 |
| 14.00 | 0.2 | 95.0 | 5.0 |
| 14.10 | 0.2 | 10.0 | 90.0 4 --> |
| 18.00 | 0.2 | 10.0 | 90.0 |
8) mass spectroscopy, antistaling agent standard solution is respectively adopted flow injection direct injected, compound parent ion is determined by full scan, again parent ion is carried out second order ms scanning, obtain fragment ion, by optimizing S-Lens, the parameters such as collision energy are optimized, obtain second order ms figure, obtain quota ion pair, qualitative ion pair, S-lens voltage, collision voltage, scan pattern and retention time, the quota ion of thiophanate-methyl is to for 343, 113/151, 074, qualitative ion pair is 343, 131/118, 123, S-lens voltage is 76V, collision voltage is 18；51, scan pattern is positive, and retention time is 7.6min, and ion source is electric spray ion source, scan mode is positive and negative switched scan, detection mode is multiple-reaction monitoring, and capillary temperature is 350 DEG C, and evaporating temperature is 300 DEG C, electron spray voltage is+3500 (-3000) V, sheath gas is 30arb, and assisted gas is 10arb, and collision gas is argon；
9) Instrument measuring, the program of sample feeding is: reagent blank, standard working curve, sample blank, sample add and actual sample, repeats above step；
10) quantitative approach, by step 9) sample introduction, with chromatographic work station Criterion working curve, sample adopts working curve quantitative。
Embodiment 3
The detection method of thiophanate-methyl residual quantity in a kind of Fructus Mali pumilae, step is as follows:
1) preparation of standard reserving solution, accurately weigh thiophanate-methyl standard substance 10mg with 100,000/balance in beaker, be accurate to 0.1mg, add acetonitrile and dissolve and be settled in 10mL volumetric flask, it is configured to the list mark storing solution that concentration is 1000 μ g/mL, 4 DEG C of preservations in refrigerator；
2) preparation of standard working solution, accurately pipette 1mL mono-mark storing solution and be placed in the brown volumetric flask of 100mL, it is settled to scale with acetonitrile, it is made into the standard intermediate liquid of 10 μ g/mL, pipette appropriate standard intermediate liquid as required, the standard working solution of 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL it is diluted to acetonitrile-aqueous solution, wherein acetonitrile-aqueous solution is containing 0.15% formic acid, in acetonitrile-aqueous solution, acetonitrile is 1:1 with the volume ratio of water, and various standard solution seal and are stored in 4 DEG C of refrigerators；
3) prepared by sample, takes 1000g belt leather Fructus Mali pumilae sample and chooses a certain amount of sample, size-reduced or tissue mashing machine's homogenate through quartering, obtain testing sample, loading in sample sack, in sealing, labelling, 4 DEG C of refrigerators, cold preservation is stand-by, if the long period that need to keep sample can-18 DEG C of freezen protective；
4) sample extraction, takes testing sample 1g, adds the ether of 6 times amount, supersound extraction 9min again after vortex oscillation 3min, adds 3g sodium chloride, is vortexed again for the centrifugal 11min of 5min, 580r/min；Divide 2 times again and add 9 times amount ether, the centrifugal 14min of 5800r/min after vortex oscillation 6min, merge organic facies, and adopt Parallel evaporator to carry out first time concentration, it is thus achieved that once concentration liquid；
5) sample elution, activated carbon pillar is first activated with eluent, uses elution after then once concentration liquid is poured into activated carbon pillar, it is thus achieved that eluting collects liquid, described eluent is the equal-volume mixed liquor of ethyl acetate and acetone, and consumption is 11 times that once concentration liquid is long-pending；
6) secondary concentration and filtration, collects eluting liquid and adopts the mode that nitrogen blows promotion eluent volatilization to carry out second time concentration, it is thus achieved that secondary concentration liquid, secondary concentration liquid adopts methanol constant volume to 2ml, adopting 0.30 μm of membrane filtration, it is thus achieved that filtrate, filtrate feed flow matter combined instrument measures；
7) chromatographic determination, chromatographic column is HypersilGOLDC18,1.9 μm, 2.1mm × 50mm, and column temperature is 35 DEG C, and sample size is 2 μ L, adopts gradient elution, and condition of gradient elution is as follows:
| Time (min) | Flow velocity (ml/min) | Acetonitrile (%) | Water (%) containing 0.15% formic acid |
| 0.00 | 0.2 | 10.0 | 90.0 |
| 2.00 | 0.2 | 10.0 | 90.0 |
| 11.00 | 0.2 | 95.0 | 5.0 |
| 14.00 | 0.2 | 95.0 | 5.0 |
| 14.10 | 0.2 | 10.0 | 90.0 |
| 18.00 | 0.2 | 10.0 | 90.0 |
8) mass spectroscopy, antistaling agent standard solution is respectively adopted flow injection direct injected, compound parent ion is determined by full scan, again parent ion is carried out second order ms scanning, obtain fragment ion, by optimizing S-Lens, the parameters such as collision energy are optimized, obtain second order ms figure, obtain quota ion pair, qualitative ion pair, S-lens voltage, collision voltage, scan pattern and retention time, the quota ion of thiophanate-methyl is to for 343, 113/151, 074, qualitative ion pair is 343, 131/118, 123, S-lens voltage is 76V, collision voltage is 18；51, scan pattern is positive, and retention time is 7.6min, and ion source is electric spray ion source, scan mode is positive and negative switched scan, detection mode is multiple-reaction monitoring, and capillary temperature is 350 DEG C, and evaporating temperature is 300 DEG C, electron spray voltage is+3500 (-3000) V, sheath gas is 30arb, and assisted gas is 10arb, and collision gas is argon；
9) Instrument measuring, the program of sample feeding is: reagent blank, standard working curve, sample blank, sample add and actual sample, repeats above step；
10) quantitative approach, by step 9) sample introduction, with chromatographic work station Criterion working curve, sample adopts working curve quantitative。
This method range of linearity is 2ng/mL～100ng/mL, test result indicate that thiophanate-methyl its concentration and peak area in this range of linearity are good linear relationship。
It is calculated as follows in sample antistaling agent content:
In formula: X is the residual quantity of antistaling agent in sample, unit is ng/kg (μ g/kg)；C is obtained the concentration of antistaling agent in sample liquid by standard working curve, and unit is nanograms per milliliter (ng/mL)；V is sample liquid constant volume, and unit is milliliter (mL)；M is sample weighting amount, and unit is gram (g)。
Above the better embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, it is also possible under the premise without departing from present inventive concept, make various change。
Claims (5)
1. the detection method of thiophanate-methyl residual quantity in a Fructus Mali pumilae, it is characterised in that step is as follows:
1) preparation of standard reserving solution, accurately weigh thiophanate-methyl standard substance 10mg with 100,000/balance in beaker, be accurate to 0.1mg, add acetonitrile and dissolve and be settled in 10mL volumetric flask, it is configured to the list mark storing solution that concentration is 1000 μ g/mL, 1 DEG C～4 DEG C preservations in refrigerator；
2) preparation of standard working solution, accurately pipette 1mL mono-mark storing solution and be placed in the brown volumetric flask of 100mL, it is settled to scale with acetonitrile, it is made into the standard intermediate liquid of 10 μ g/mL, pipette appropriate standard intermediate liquid as required, be diluted to the standard working solution of 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL with acetonitrile-aqueous solution, various standard solution seal and are stored in 1 DEG C～4 DEG C refrigerators；
3) prepared by sample, takes 1000g belt leather Fructus Mali pumilae sample and chooses a certain amount of sample, size-reduced or tissue mashing machine's homogenate, it is thus achieved that testing sample through quartering, loads in sample sack, and in sealing, labelling, 1 DEG C～4 DEG C refrigerators, cold preservation is stand-by；
4) sample extraction, takes testing sample, adds the ether of 5～8 times amount, supersound extraction 8～10min again after vortex oscillation 2～3min, adds 2～4g sodium chloride, is vortexed again for 4～5min, and 5500～6000r/min is centrifuged 10～12min；Divide 2 times again and add 8～10 times amount ether, the centrifugal 12～15min of 5500～6000r/min after vortex oscillation 6～7min, merge organic facies, and adopt Parallel evaporator to carry out first time concentration, it is thus achieved that once concentration liquid；
5) sample elution, activated carbon pillar is first activated with eluent, uses elution after then once concentration liquid is poured into activated carbon pillar, it is thus achieved that eluting collects liquid, described eluent is the equal-volume mixed liquor of ethyl acetate and acetone, and consumption is 10～12 times that once concentration liquid is long-pending；
6) secondary concentration and filtration, collects eluting liquid and adopts the mode that nitrogen blows promotion eluent volatilization to carry out second time concentration, it is thus achieved that secondary concentration liquid, secondary concentration liquid adopts methanol constant volume to 2ml, adopting 0.30 μm of membrane filtration, it is thus achieved that filtrate, filtrate feed flow matter combined instrument measures；
7) chromatographic determination；
8) mass spectroscopy；
9) Instrument measuring, the program of sample feeding is: reagent blank, standard working curve, sample blank, sample add and actual sample, repeats above step；
10) quantitative approach, by step 9) sample introduction, with chromatographic work station Criterion working curve, sample adopts working curve quantitative。
2. the detection method of thiophanate-methyl residual quantity in Fructus Mali pumilae according to claim 1, it is characterised in that step 2) in, acetonitrile-aqueous solution is containing 0.15% formic acid, and in acetonitrile-aqueous solution, acetonitrile is 1:1 with the volume ratio of water。
3. the detection method of thiophanate-methyl residual quantity in Fructus Mali pumilae according to claim 1 and 2, it is characterized in that, step 8) in, the quota ion of thiophanate-methyl is to for 343,113/151,074, qualitative ion pair is 343,131/118,123, S-lens voltage is 76V, and collision voltage is 18；51, scan pattern is positive, and retention time is 7.6min, and ion source is electric spray ion source, scan mode is positive and negative switched scan, detection mode is multiple-reaction monitoring, and capillary temperature is 350 DEG C, and evaporating temperature is 300 DEG C, electron spray voltage is+3500 (-3000) V, sheath gas is 30arb, and assisted gas is 10arb, and collision gas is argon。
4. the detection method of thiophanate-methyl residual quantity in Fructus Mali pumilae according to claim 3, it is characterised in that step 7) in, chromatographic column is HypersilGOLDC18, and thickness is 1.9 μm, and internal diameter is 2.1mm × 50mm, column temperature is 35 DEG C, and sample size is 2 μ L, adopts gradient elution。
5. the detection method of thiophanate-methyl residual quantity in Fructus Mali pumilae according to claim 4, it is characterised in that step 7) in condition of gradient elution as follows:
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| CN106840797A (en) * | 2017-01-24 | 2017-06-13 | 上海析维医疗科技有限公司 | The automatic preparation work station and compound method of a kind of standard liquid |
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