CN109001328A - A kind of LC-MS/MS detection method of polyoxin B - Google Patents
A kind of LC-MS/MS detection method of polyoxin B Download PDFInfo
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- CN109001328A CN109001328A CN201810938087.5A CN201810938087A CN109001328A CN 109001328 A CN109001328 A CN 109001328A CN 201810938087 A CN201810938087 A CN 201810938087A CN 109001328 A CN109001328 A CN 109001328A
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Abstract
The invention discloses a kind of LC-MS/MS detection methods of polyoxin B.The present invention is first according to the properities optimization instrument condition of polyoxin B, using ACQUITY UPLC BEH Amide column as chromatographic column；0.1% formic acid water and acetonitrile are mobile phase；It is measured using multiple-reaction monitoring (MRM) positive ion mode.The present invention is experimentally confirmed: within the scope of 0.002~0.2mg/L, polyoxin B linear relationship is good, and the rate of recovery is 97.2%~104.3%, relative standard deviation 0.5%.Institute's construction method is fast and convenient, accuracy and high sensitivity, can be used for the detection of the quality control and pesticide residue of Pesticidal products.Another selection is provided for the sensitive, quick of polyoxin B, Accurate Determining.
Description
Technical field
The present invention relates to a kind of LC-MS/MS detection methods of polyoxin B, belong to Pesticides Testing technical field.
Background technique
Polyoxin, English common name Polyoxin, also known as polyoxin, multi-effect mycin, Pola peace, Poly mycin belong to
Less toxic absorbability peptide pyrimidine nucleotide antibiotics fungicide, mechanism of action is: the life of interference pathogen cell wall chitin
Object synthesizes so as to cause cell death.It is mainly used for preventing and treating wheat powdery mildew, rice sheath blight disease, cucumber downy mildew, melon withered
A variety of fungal diseases such as disease, alternaria leaf spot of apple, strawberry and grape grey mould, black fleck disease of ginseng and Pear black spot.More anti-mildews
Procatarxis its low toxicity, efficiently, broad spectrum activity become use scope so far is most wide, the most successful important farm antibiotics of exploitation it
One, it is used widely in agricultural production.
Japanese Innovation Input uses polyoxin earliest, and effective component is by cocoa streptomysin A Su mutation
The metabolin polyoxin B that (Stroptomyces cacaoi var.asoensis) is generated.At present to the analysis of polyoxin B
Method mainly has microbial method, liquid chromatography and Capillary Electrophoresis --- electrogenerated chemiluminescence method, wherein being using more
Liquid chromatography is (such as: 1, Chinese patent CN103776929A, a kind of denomination of invention: high performance liquid chromatography detection polyoxin B
Method；2, in welfare, Song Xifeng, Jiang Jun, etc..HPLC analytical method [J] pesticide of polyoxin B, 2008,
47(3):188-189).Although high performance liquid chromatography can detecte polyoxin B, but polyoxin B and more anti-mildews first
Plain homologue structure is similar, and the interference by homologue is easy in HPLC detection；Secondly, HPLC chromatogram poor sensitivity, Bu Nengshi
Answer the residual requirement of existing agriculture.
Through retrieving, so far both at home and abroad there is not yet the report of polyoxin B LC-MS analysis method.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of LC-MS/MS detection methods of polyoxin B.The present invention is according to more
The property of antimycin B obtains the ion pair of higher response with cation scan pattern, has selected have good reservation to it
Chromatographic column, optimize chromatographic condition and mass spectrometry parameters, establish the LC-MS detection method of polyoxin B, to be more
The sensitive, quick of antimycin B, Accurate Determining provide another selection.
The technical scheme is that a kind of LC-MS/MS detection method of polyoxin B, characterized in that
1) preparation of prepare liquid
By determinand plus water, polyoxin B is made to be dissolved in the water, methanol-water is then added, and (volume ratio of methanol and water is
6-8:2-4, preferably 7:3) dilution after be used as liquid to be detected；
2) the LC-MS/MS detection of polyoxin B
Using ACQUITY UPLC BEH Amide column as chromatographic column；0.1% formic acid water and acetonitrile are mobile phase；Using mostly anti-
It is qualitative and quantitative that (MRM) positive ion mode progress LC-MS/MS should be monitored.
Its chromatographic condition are as follows: flow velocity: 0.25mL/min；Column temperature: 40 DEG C；Sample volume: 1 μ L.
Mobile phase: 0.1% formic acid water and acetonitrile；Gradient elution program: 80% acetonitrile when 0min；0.5~4min linearly subtracts
As low as 50% acetonitrile；4~5min is linearly decreased to 40% acetonitrile；5.5min increases to 80% acetonitrile, carries out system balancing later.
Its Mass Spectrometry Conditions is as follows:
Electron spray (ESI) ion source, cation scan pattern；Capillary voltage: 4.0kV；Dry temperature degree: 300 DEG C；It is dry
Pathogenic dryness flow velocity: 8L/min；Sheath temperature degree: 350 DEG C；Sheath gas: 11L/min；Photoelectric multiplier voltage: 300V.Monitoring pattern
Using more reaction detection modes (MRM).The mass spectrometry parameters of determinand molecular ion and fragment ion are shown in Table 1.Using
MassHunter software carries out data analysis.
1 Mass Spectrometry Conditions parameter of table
*: quota ion pair.
Further, the present invention calculates the content of polyoxin B, standard curve y=248.09x- using external standard method
160.82 correlation coefficient r=0.9991.
The beneficial effects of the present invention are:
1, the present invention establishes a kind of LC-MS/MS detection method of polyoxin B for the first time
The present invention is first according to the properities optimization instrument condition of polyoxin B, with ACQUITY UPLC BEH Amide column
For chromatographic column；0.1% formic acid water and acetonitrile are mobile phase；It is measured using multiple-reaction monitoring (MRM) positive ion mode.Polyoxin
B obtains good reservation in BEH Amide chromatographic column, while the chromatographic column is compared with other polarity chromatographic columns, to salt
There are the separation for being conducive to determinand and matrix for minimum living.
2, detection effect is good
The present invention is experimentally confirmed: within the scope of 0.002~0.2mg/L, the good (r of polyoxin B linear relationship2=
0.9997), the rate of recovery is 97.2%~104.3%, relative standard deviation 0.5%.Institute's construction method is fast and convenient, accuracy and
High sensitivity can be used for the detection of the quality control and pesticide residue of Pesticidal products.For the sensitive, quick, accurate of polyoxin B
Measurement provides another selection.
3, HPLC is compared, the present invention is more suitable for Detecting Pesticide
Firstly, the present invention is optimized by Mass Spectrometry Conditions, the molecular ion and fragment for obtaining signal stabilization, having higher response
Ion can eliminate the interference of the substances such as polyoxin homologue；Secondly, method quantitative limit of the invention reaches 2 μ g/L, spirit
Sensitivity is high；3) detection speed is fast, more efficient；Therefore, method of the invention is more suitable for the trace detection of pesticide residue.
Detailed description of the invention
Fig. 1 is the total ion of MRM of polyoxin B standard items and the ion stream chromatogram of selection ion；
Fig. 2 is the chromatogram that BEH Hilic chromatographic column and BEH Amide detect polyoxin B；Wherein A:BEH Hilic
The chromatogram that chromatographic column obtains, Hilic chromatographic column be waters exploitation widely used chromatographic column, B: the BEH of this method
The chromatogram that Amide is obtained；The two is compared, and chromatographic column used in this method has better reservation, and peak shape sharply has higher spirit
Sensitivity；
Fig. 3 is the mass spectrogram of polyoxin B；
Fig. 4 is the canonical plotting of polyoxin B.
Specific embodiment
1. experimental section
1.1 instruments and reagent
HP1290 high performance liquid chromatograph (Agilent company of the U.S.)；Agilent 6460LC-QQQ mass spectrograph (U.S.'s peace
Jie Lun company).Agilent Masshunter work station.Millipore ultrapure water production system.Chromatographic column: ACQUITY UPLC
BEH Amide column (100 × 2.1mm, 1.7 μm)；Miillpore filter: 0.22 μm of organic film.
Polyoxin Polyoxin B (purity 84.4%) is provided by Japanese scientific research Co., Ltd.；Acetonitrile (chromatographically pure)；First
Alcohol (chromatographically pure)；Ultrapure water (resistivity 18.2M Ω cm, 25 DEG C).
1.2 chromatographic condition
Chromatographic column: ACQUITY UPLC BEH Amide (100mm × 2.1mm, 1.7 μm), flow velocity: 0.25mL/min；Column
Temperature: 40 DEG C；Sample volume: 1 μ L.
Mobile phase: 0.1% formic acid water and acetonitrile；Gradient elution program: 80% acetonitrile (20% 0.1% formic acid when 0min
Water)；0.5~4min is linearly decreased to 50% acetonitrile (50% 0.1% formic acid water)；4~5min is linearly decreased to 40% second
Nitrile (60% 0.1% formic acid water)；5.5min increases to 80% acetonitrile, carries out system balancing later.
1.3 Mass Spectrometry Conditions
Electron spray (ESI) ion source, cation scan pattern；Capillary voltage: 4.0kV；Dry temperature degree: 300 DEG C；It is dry
Pathogenic dryness flow velocity: 8L/min；Sheath temperature degree: 350 DEG C；Sheath gas: 11L/min；Photoelectric multiplier voltage: 300V.Monitoring pattern
Using more reaction detection modes (MRM), the mass spectrometry parameters of determinand molecular ion and fragment ion are shown in Table 1.Using
MassHunter software carries out sample analysis.
1.4 determination step
1.4.1 the preparation of standard solution
Polyoxin Polyoxin B standard product 0.0119g is accurately weighed (accurately to 0.0001g) in 10mL volumetric flask.
After adding 5ml ultrapure water to dissolve, with methanol constant volume to scale, shake up spare.This is polyoxin B stock solution, and mass fraction is
1.0mg/kg is placed in 4 DEG C of refrigerators and saves.Again with methanol-water (70:30) solution is diluted to the mark of appropriate mass concentration when use
Quasi- working solution.
1.4.2 the preparation of sample solution
10% Wettable polyoxin powder 0.0100g is accurately weighed (accurately to the sample of 0.0001g) in 100mL capacity
In bottle.It is dissolved with 10ml water, scale is settled to methanol-water (70:30) solution, is shaken up as reserve liquid.Draw reserve liquid 1mL
In another 100mL volumetric flask, it is settled to scale with methanol-water (70:30) solution, with 0.22 μm of aperture filter membrane mistake after shaking up
Filter collects filtrate and waits for machine testing.
1.4.3 analysis measurement
Under above-mentioned instrument condition, after instrumental baseline is stablized, several needle standard specimen solutions are continuously injected into up to the peak of adjacent 2 needle
After area change is less than 1.5%, measured by the sequence sample introduction of standard solution, sample solution, sample solution, standard solution, with outer
Mark method calculates separately the content of polyoxin B.Polyoxin B standard chromatogram is shown in Fig. 1.
2. results and discussion
The selection of 2.1 chromatographic columns
It is mostly C18, C8, nh 2 column, phenyl column etc. that Pesticides Testing liquid chromatogram, which separates common chromatographic column, the study show that
Since polyoxin molecular polarity is soluble easily in water by force, organic solvent is not dissolved in.Its molecular structure contains 2 amino, 1 carboxyl.
Do not retain in the chromatographic columns such as common reverse-phase chromatographic column C18, C8.We have attempted color of several moneys for separating polar substance
Compose column, the results showed that polyoxin B obtains good reservation (as shown in Figure 2), while the color in BEH Amide chromatographic column
Column is composed compared with other polarity chromatographic columns, there are the separation for being conducive to determinand and matrix to the minimum living of salt.
The selection of 2.2 chromatogram flow phases
Liquid chromatogram mobile phase mostly uses methanol and acetonitrile.In the method, acetonitrile is eluting solvent more weaker than methanol,
It is more advantageous to the reservation of determinand on a column.In addition polyoxin B is stablized in acid and neutral solution, in alkaline solution
In easily decompose, in addition under the conditions of low pH mobile phase inhibit carboxyl ionization, increase polyoxin B retain while can improve mass spectrum
Response.It is finally used by condition optimizing using+0.1% formic acid water of acetonitrile as mobile phase.
The optimization of 2.3 condition of gradient elution
By the optimization discovery to mobile phase elution process, when using isocratic elution, the retention time of polyoxin B is long,
Chromatographic peak is wider, and the sensitivity of large effect detection is unfavorable for accurate quantitative analysis.Using gradient elution, it is sharp right to have obtained
The peak shape of title, hence it is evident that improve the sensitivity of method.The salts substances that minimum living is stayed can first be rushed with initial Weak solvent simultaneously
Chromatographic column out is discharged to waste liquid by software control effluent to reduce to the mass spectrographic pollution in rear end.
The optimization of 2.4 Mass Spectrometry Conditions
Polyoxin B in ESI (+) mode full scan mass spectrum with [M+H]+Quasi-molecular ion peak is stabilized, and m/z is
508.1.In order to improve ionising effect, this experiment is respectively to mass spectrographic capillary voltage, photoelectric multiplier voltage, dry temperature
Degree and flow velocity, the instrument conditions such as the temperature of sheath gas and flow velocity optimize.Point that signal stabilization has finally been determined, has had higher response
Daughter ion and fragment ion.Mass spectrogram is as shown in Figure 3.
The production of 2.5 standard curves
Accurately pipette polyoxin B stock solution, successively diluted with mobile phase, be configured to 0.002,0.005,0.010,
0.02, the standard solution of 0.050,0.100,0.200mg/L, with the peak area of polyoxin B and mass concentration for longitudinal and transverse seat
Mark is drawn linear relationship curve (see Fig. 4).As a result it is y=248.09x-160.82, correlation coefficient r that equation of linear regression, which can be obtained,
=0.9991, show within the scope of 0.002~0.200mg/L, the mass concentration (x) and peak area (y) of polyoxin B are linearly closed
System is good, is suitble to do quantitative analysis.Using 3 times of signal-to-noise ratio as detection limit, 10 times of signal-to-noise ratio measure this method as quantitative limit
Instrument detection limit and quantitative limit are respectively 0.5 μ g/L and 2.0 μ g/L, and it is higher to show that this method has the detection of polyoxin B
Sensitivity.
The measurement of 2.6 actual samples
5 samples are accurately weighed from same a 10% Wettable polyoxin powder product, at aforementioned 1.42 method
It after reason, is analyzed under these experimental conditions, calculates polyoxin B mass fraction and relative standard is inclined, the results are shown in Table 2.5
Relative standard deviation RSD≤10% of parallel sample measurement result, illustrates this method suitable for Wettable polyoxin powder
The measurement of polyoxin B content.
The precision experiment result of 2 polyoxin of table
3 conclusions
This research establishes sensitive, the accurate LC-MS method of measurement polyoxin B content for the first time.Pass through mass spectrum item
Piece optimization, the molecular ion and fragment ion for obtaining signal stabilization, having higher response.It has selected and has been more suitable for polyoxin B point
The BEH Amide chromatographic column of analysis, optimizes chromatographic separation condition, has obtained sharp, symmetrical chromatographic peak.Method validation result table
Bright this method sensitivity, preci-sion and accuracy are higher, and linear relationship is good, and quantitative limit reaches 2 μ g/L, suitable for Pesticidal products
Quality control, while the residue detection for the drug from now on provides better choice.
Claims (6)
1. a kind of LC-MS/MS detection method of polyoxin B, characterized in that
1) preparation of prepare liquid
By determinand plus water, polyoxin B is made to be dissolved in the water, is used as liquid to be detected after methanol-water solution dilution is then added；
The volume ratio of methanol and water is 6-8:2-4 in methanol-water solution；
2) the LC-MS/MS detection of polyoxin B
Using ACQUITY UPLC BEH Amide column as chromatographic column；0.1% formic acid water and acetonitrile are mobile phase；Using more reaction prisons
It is qualitative and quantitative to survey positive ion mode progress LC-MS/MS.
2. a kind of LC-MS/MS detection method of polyoxin B as described in claim 1, characterized in that its chromatographic column uses
Gradient elution, gradient elution program: 80% acetonitrile when 0min；0.5~4min is linearly decreased to 50% acetonitrile；4~5min, line
Property is decreased to 40% acetonitrile；5.5min increases to 80% acetonitrile, carries out system balancing later.
3. a kind of LC-MS/MS detection method of polyoxin B as claimed in claim 2, characterized in that the chromatographic condition
It is flow velocity: 0.25mL/min；Column temperature: 40 DEG C；Sample volume: 1 μ L.
4. a kind of LC-MS/MS detection method of polyoxin B as described in any one of claim 1-3, characterized in that
Its Mass Spectrometry Conditions is as follows: electron spray ESI ion source, cation scan pattern；Capillary voltage: 4.0kV；Dry temperature degree: 300
℃；Dry gas stream speed: 8L/min；Sheath temperature degree: 350 DEG C；Sheath gas: 11L/min；Photoelectric multiplier voltage: 300V；Monitoring
Mode uses more reaction detection mode MRM.
5. a kind of LC-MS/MS detection method of polyoxin B as claimed in claim 4, characterized in that polyoxin B molecule
The mass spectrometry parameters of ion and fragment ion see the table below；
*: quota ion pair.
6. a kind of LC-MS/MS detection method of polyoxin B as claimed in claim 5, characterized in that use external standard method meter
Calculate the content of polyoxin B, standard curve y=248.09x-160.82, correlation coefficient r=0.9991.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109765315A (en) * | 2019-01-30 | 2019-05-17 | 陕西麦可罗生物科技有限公司 | A kind of preparation method and detection method of polyoxin component C |
| CN111307965A (en) * | 2019-12-16 | 2020-06-19 | 陕西麦可罗生物科技有限公司 | Method for detecting polyoxin M by high performance liquid chromatography |
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| US20050080260A1 (en) * | 2003-04-22 | 2005-04-14 | Mills Randell L. | Preparation of prodrugs for selective drug delivery |
| CN106546672A (en) * | 2016-10-18 | 2017-03-29 | 吉林农业大学 | A kind of residue analysis method of polyoxin on ginseng |
| CN107153101A (en) * | 2017-04-24 | 2017-09-12 | 上海市农业科学院 | A kind of detection method of plant-derived feed polyoxin |
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2018
- 2018-08-17 CN CN201810938087.5A patent/CN109001328A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050080260A1 (en) * | 2003-04-22 | 2005-04-14 | Mills Randell L. | Preparation of prodrugs for selective drug delivery |
| CN106546672A (en) * | 2016-10-18 | 2017-03-29 | 吉林农业大学 | A kind of residue analysis method of polyoxin on ginseng |
| CN107153101A (en) * | 2017-04-24 | 2017-09-12 | 上海市农业科学院 | A kind of detection method of plant-derived feed polyoxin |
Non-Patent Citations (3)
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| TORU ARAKAWA等: "Insecticidal effect of a fungicide containing polyoxin B on the larvae of Bombyx mori (Lepidoptera: Bombycidae), Mamestra brassicae, Mythimna separata, and Spodoptera litura (Lepidoptera: Noctuidae)", 《APPLIED ENTOMOLOGY AND ZOOLOGY》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109765315A (en) * | 2019-01-30 | 2019-05-17 | 陕西麦可罗生物科技有限公司 | A kind of preparation method and detection method of polyoxin component C |
| CN111307965A (en) * | 2019-12-16 | 2020-06-19 | 陕西麦可罗生物科技有限公司 | Method for detecting polyoxin M by high performance liquid chromatography |
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Application publication date: 20181214 |