CN107462652A - A kind of method of Ningnanmycin residual quantity in measure vegetable food - Google Patents
A kind of method of Ningnanmycin residual quantity in measure vegetable food Download PDFInfo
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Abstract
The invention belongs to technical field of food safety, is related to a kind of method for determining Ningnanmycin residual quantity in vegetable food.Weigh homogeneous sample, extracted with acidified methanol solution (pH=4.5) homogeneous, anhydrous magnesium sulfate and PSA adsorptive hindrance things, after high speed refrigerated centrifuge, supernatant is rotated near dry, water dissolved residue, HLB purification column purifications are crossed, elution liquid nitrogen is blown to dry, flowing phased soln constant volume, it is to be measured through 0.22 μm of organic membrane filtration.Determinand detects through LC-MS instrument, quantified by external standard method.Detection method pre-treatment step of the present invention is simply novel, good impurity removing effect, and the sensitivity of method, the rate of recovery are high, and the precision of measurement result is good, can effectively detect Ningnanmycin residual quantity in all kinds of fruits and vegetables, grain.
Description
Technical field
The invention belongs to technical field of food safety, and in particular to a kind of Liquid Chromatography-Tandem Mass Spectrometry measure fruits and vegetables, grain
The method of middle Ningnanmycin residual quantity.
Technical background
Ningnanmycin is a kind of Cystosine nucleocide type antibiotics, is white powder, 195 DEG C of fusing point is soluble in water, can
Methanol is dissolved in, is slightly soluble in ethanol, is insoluble in the organic solvents such as acetone, ethyl ester, benzene, pH3.0-5.0 is relatively stable, easy in alkalescence
Decomposition loses activity.
Ningnanmycin is Chengdu Inst. of Biology, Chinese Academy of Sciences after the Seventh Five-Year Plan, 85,95 National Key Research Programs and ground
Successful patented technology product is made, at present in tobacco mosaic virus disease, tomato virus disease, pepper virus disease, rice seedling blight, big
Beans root rot, stripe disease, alternaria leaf spot of apple, registration is achieved in powdery mildew of cucumber.Moral Johnson ＆ Johnson thing share has
Limit company produces successfully to Ningnanmycin pesticide industry metaplasia, developed 2% aqua, 8% aqua, 10% soluble powder,
The Ningnanmycin series of products such as bitter peaceful seed coat agent, are widely applied, market potential in nuisanceless fruits and vegetables field of planting
It is rice and wheat, the absolute usable floor area of Ningnanmycin is still inestimable.Because Ningnanmycin product patent arrived in 2013
Phase, it is contemplated that manufacturer can be more and more from now on, and its production capacity, which has, to be obviously improved, and also can significantly increase in the application of planting industry
Add.
Ningnanmycin is to large and small mouse acute oral LD50For 5492~6845 mg/kgs, the percutaneous LD of chmice acute50＞
1000 mg/kgs, in use in the presence of certain medicament residue.《GB 2763-2014 national food safety standard food
Pesticides MRL》In increased the MRL standard of Ningnanmycin newly, it is specified that Ningnanmycin faces in brown rice
When limitation be 0.2mg/kg, it is 1mg/kg to be limited the quantity temporarily in apple.
But at present, also without the detection method for Ningnanmycin residual quantity in food.In food security increasingly
On the premise of receiving significant attention, the detection method of Ningnanmycin in a kind of necessary vegetable food of exploitation.
This law is according to the chemical characteristic of Ningnanmycin, preferably Extraction solvent and purification style.Ningnanmycin polarity is larger,
Water polar solvent is dissolved in, this law compares the extractants such as water, methanol, acetonitrile, and preferably its suitable pH value range, final true
Recognizing acidified methanol (acetic acid regulation methanol adjusts pH to 4.5), extraction efficiency is high, and Ningnanmycin can be stabilized in the extractant.
For the endogenous chaff interference such as various pigments, aliphatic acid in vegetable food, develop in extraction process with anhydrous magnesium sulfate and
PSA adsorpting pigments and aliphatic acid, the means then further purified with HLB solid-phase extraction columns again.
Detection method pre-treatment step of the present invention is simply novel, good impurity removing effect, the sensitivity of method, the rate of recovery
Height, the precision of measurement result is good, and detection limit is low, can effectively detect Ningnanmycin residual quantity in all kinds of fruits and vegetables, grain.
The content of the invention
The technical problems to be solved by the invention apply to the detection method of Ningnanmycin residual quantity in vegetable food,
The Ningnanmycin remained in vegetable food can be effectively extracted, and removes chaff interference well.Detection limit can meet country
Requirement of the standard to Ningnanmycin MRL in rice and apple.
The technical scheme is that realized by following steps：
(1) extract：Homogeneous sample 10g is weighed in 50mL centrifuge tubes, the acetate-methanol for adding 30mL pH=4.5 is molten
Liquid, homogeneous extract, and after 8000r/min refrigerated centrifuges, pour out supernatant, residue is molten with 20mL pH=4.5 acetate-methanol again
Liquid repeats extraction once, merges supernatant, adds 6g anhydrous magnesium sulfates and 150mgPSA, shakes, transfer supernatant to revolving bottle
In, 40 DEG C of revolvings are done near, pipette 5mL water dissolved residues, stand-by.
(2) purify：HLB decontaminating columns are activated with 5mL methanol, 5mL water respectively before use, and above-mentioned solution is crossed into HLB decontaminating columns
Purification；5mL water cleaning revolving bottle is pipetted again, and cleaning fluid crosses HLB purification column purifications, and loading process maintains 1 drop/sec；By decontaminating column
After draining, pipette 5mL methanol elution, collect eluent in 10mL centrifuge tubes, 40 DEG C of nitrogen be blown to it is dry, pipette 2mL flowing mix
Residue is solved, after mixing, crosses 0.22 μm of filter membrane, it is to be measured.
(3) determine：Standard liquid and sample treatment solution are measured under the conditions of following Liquid Chromatography-Tandem Mass Spectrometries：
Chromatographic column：C18,1.7 μm, 2.1mm × 50mm
Mobile phase：5mmol/L ammonium acetate solutions, acetonitrile
Flow velocity：0.4mL/min；
Sample size：5.0μL；
Column temperature：40℃；
Gradient elution is shown in Table 1
The gradient elution of table 1
Mass Spectrometry Conditions：
Ion gun：ESI electric spray ion sources；
Scan mode：Cation scans；
Detection mode：MRM multiple-reaction monitorings；
Ion source temperature：120℃；
Remove solvent temperature：450℃
Ion pair, taper hole voltage, collision energy are shown in Table 2.
The ion pair of table 2, taper hole voltage, collision energy
With respect to the maximum allowable offset of abundance of ions during qualitative confirmation：
Relative ion abundance ＞ 50%, it is allowed to relative deviation ± 20%
20% ＜ relative ion abundance≤50%, it is allowed to relative deviation ± 25%
10% ＜ relative ion abundance≤20%, it is allowed to relative deviation ± 30%
Relative ion abundance≤10%, it is allowed to relative deviation ± 50%
(4) judge
Using mass concentration x as abscissa, peak area y is ordinate, draws 5 standard working curves, is worked with standard bent
Line quantifies to sample, and the response of Ningnanmycin should be in the range of linearity that instrument detects in sample solution；In above-mentioned instrument
Under the conditions of device, with the presence or absence of Ningnanmycin, it is necessary to meet following condition in judgement sample：The chromatographic peak occurred in sample solution is protected
Stay the time consistent with standard working solution, it is allowed to which deviation is less than ± 2.5%, and the relative abundance of the chromatographic peak ion pair is suitable with concentration
Standard working solution relative abundance it is consistent, relative abundance deviation is no more than above-mentioned regulation, then can determine that containing Ningnanmycin.
(5) result calculates：
Ningnanmycin residual quantity is calculated by formula (1) in sample, and result of calculation need to deduct blank value.
In formula：
The content of Ningnanmycin residual quantity in X- samples, unit are ng/kg (μ g/kg)；
CSampleThe concentration that Ningnanmycin remains in-sample solution, unit is nanograms per milliliter (ng/mL)；
F- intermediate dilute multiples；
The final constant volumes of V-, unit are milliliter (mL)；
M- sample qualities, unit are gram (g).
(6) method detection limit：
Detection method pre-treatment step of the present invention is simply novel, good impurity removing effect, the sensitivity of method, the rate of recovery
Height, the precision of measurement result is good, and when blank sample adds 10 μ g/kg Ningnanmycins, signal to noise ratio is ＞ 10, therefore our standard measure
It is limited to：10 μ g/kg, during signal to noise ratio=3, this method detection is limited to 3 μ g/kg.
Brief description of the drawings
Fig. 1 is 10 μ g/kg Ningnanmycin sample mark-on signal to noise ratio chromatograms
Fig. 2 is 250ng/ml Ningnanmycin standard liquid chromatograms
Specific implementation method
The present invention will be described further by following examples.Embodiment is merely to illustrate the present invention rather than limitation
The scope of the present invention.Unless otherwise defined, all specialties used in text and scientific words and one skilled in the art institute are ripe
The meaning known is identical.In addition, any method similar or impartial to described content and material all can be used in the present invention, Wen Zhong
Described preferable implementation, which only presents a demonstration, to be used.
Embodiment 1
1st, instrument and reagent
High performance liquid chromatography-tandem mass instrument：U.S. Waters, UPLC-Xevo TQ；
Standard substance：Ningnanmycin, purity 98.5%；
Methanol, ammonium acetate：Chromatographically pure；
Acetic acid is pure to analyze；
Anhydrous magnesium sulfate is pure to analyze；
PSA is pure to analyze；
HLB solid phase extraction columns：6mL, 200mg；
Water used is one-level water in this method.
2nd, instrumental conditions
Liquid phase chromatogram condition：
Chromatographic column：Waters, BEH C18,1.7 μm, 2.1mm × 50mm
Mobile phase：5mmol/L ammonium acetate solutions, acetonitrile
Flow velocity：0.4mL/min；
Sample size：5.0μL；
Column temperature：40℃；
Gradient elution is shown in Table 1
The gradient elution of table 3
| A：5mmol/L ammonium acetate solutions | B：Acetonitrile | |
| 0.00 | 95% | 5% |
| 1.50 | 50% | 50% |
| 3.00 | 0% | 100% |
| 4.00 | 0% | 100% |
| 4.30 | 95% | 5% |
| 6.00 | 95% | 5% |
Mass Spectrometry Conditions：
Ion gun：ESI electric spray ion sources；
Scan mode：Cation scans；
Detection mode：MRM multiple-reaction monitorings；
Ion source temperature：120℃；
Remove solvent temperature：450℃
Ion pair, taper hole voltage, collision energy are shown in Table 2.
The ion pair of table 4, taper hole voltage, collision energy
3rd, linear equation and standard items chromatogram
Standard reserving solution is prepared：10.6mg Ningnanmycin standard substances are weighed, is dissolved with water and is settled to 100mL, standard
Stock concentrations are 104.4mg/L.
Standard working solution is prepared with above-mentioned standard liquid：Concentration is 0.02mg/L, 0.05mg/L, 0.2mg/L, 0.5mg/L,
1mg/L, 2mg/L.It is measured under above-mentioned chromatographic condition, quantified by external standard method.Using peak area y as ordinate, concentration x is horizontal seat
Mark carries out linear regression, as a result such as table 5
The Ningnanmycin retention time of table 5, regression equation and linearly dependent coefficient
4th, sample-pretreating method
(1) extract：The sample 10g after crushing uniformly is weighed in 50mL centrifuge tubes, the acetic acid that addition 30mL pH are 4.5-
Methanol solution, homogeneous extraction, after 8000r/min refrigerated centrifuges, pour out supernatant, residue again with the acetic acid that 20mL pH are 4.5-
Methanol solution repeats extraction once, merges supernatant, adds 6g anhydrous magnesium sulfates and 150mgPSA, shakes, and transfer supernatant is extremely
In revolving bottle, 40 DEG C of revolvings are done near, pipette 5mL water dissolved residues, stand-by.
(2) purify：HLB decontaminating columns are activated with 5mL methanol, 5mL water respectively before use, and above-mentioned solution is crossed into HLB decontaminating columns
Purification；5mL water cleaning revolving bottle is pipetted again, and cleaning fluid crosses HLB purification column purifications, and loading process maintains 1 drop/sec；By decontaminating column
After draining, pipette 5mL methanol elution, collect eluent in 10mL centrifuge tubes, 40 DEG C of nitrogen be blown to it is dry, pipette 2mL flowing mix
Residue is solved, after mixing, crosses 0.22 μm of filter membrane, it is to be measured.
5th, sample determines
6 parts of samples are weighed, samples are handled by 4 pre-treating methods, are detected by 2 instrumental conditions, during reservation
Between, abundance of ions than qualitative, quantified by external standard method.Experimental result is as shown in table 6, table 7
The measurement result of Ningnanmycin in the apple sample of table 6
The measurement result of Ningnanmycin in the rice sample of table 7
6th, precision and the rate of recovery
The precision and rate of recovery experimental result of this method are as shown in table 8.
The rate of recovery experimental result of table 8
7th, detection limit
The detection of Ningnanmycin method is limited to 3 μ g/kg, the μ g/kg of quantitative limit 10.
Claims (4)
- A kind of 1. method for determining Ningnanmycin residual quantity in vegetable food, it is characterised in that method comprises the following steps：(1) extract：Homogeneous sample 10g is weighed in 50mL centrifuge tubes, adds 30mL pH=4.5 acetate-methanol solution, homogeneous extracts, After 8000r/min refrigerated centrifuges, supernatant is poured out, residue repeats to extract one with 20mLpH=4.5 acetate-methanol solution again It is secondary, merge supernatant, add 6g anhydrous magnesium sulfates and 150mgPSA, shake, transfer supernatant is into revolving bottle, and 40 DEG C of revolvings are extremely It is near dry, 5mL water dissolved residues are pipetted, it is stand-by.(2) purify：HLB decontaminating columns are activated with 5mL methanol, 5mL water respectively before use, and above-mentioned solution is crossed into HLB purification column purifications；Pipette again 5mL water cleans revolving bottle, and cleaning fluid crosses HLB purification column purifications, and loading process maintains 1 drop/sec；After decontaminating column is drained, pipette 5mL methanol elutes, and collects eluent in 10mL centrifuge tubes, and 40 DEG C of nitrogen are blown to dry, pipette 2mL mobile phase dissolved residues, mix Afterwards, 0.22 μm of filter membrane is crossed, for liquid chromatography tandem mass spectroscopy.
- 2. a kind of method for determining Ningnanmycin residual quantity in vegetable food according to claim 1, it is characterized in that：Extraction Liquid is pH=4.5 acetate-methanol solution, and extract solution usage amount 50mL, extraction time is twice.
- 3. a kind of method for determining Ningnanmycin residual quantity in vegetable food according to claim 1, it is characterized in that：Extraction Process first uses the chaff interference such as 6g anhydrous magnesium sulfates and 150mgPSA adsorpting pigments and aliphatic acid, then is purified with 6mL, 200mg HLB Column purification.
- A kind of 4. method for determining Ningnanmycin residual quantity in vegetable food according to claim 1, it is characterized in that Ningnan The monitoring ion pair of mycin is m/z 456.8/327.3 and m/z456.8/439.5, and collision energy is respectively 17eV and 13eV, is bored Hole voltage is 30V.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108562673A (en) * | 2018-07-17 | 2018-09-21 | 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 spectrum detection method measuring Ningnanmycin content in tomato |
| CN110261509A (en) * | 2019-07-10 | 2019-09-20 | 中山永恒检测科技有限公司 | The high-efficiency liquid chromatography method for detecting of Ningnanmycin residual quantity in a kind of measurement rice |
| CN110261511A (en) * | 2019-07-16 | 2019-09-20 | 中山永恒检测科技有限公司 | The Liquid Chromatography-Tandem Mass Spectrometry detection method of Ningnanmycin residual quantity in a kind of cucumber |
| CN111024854A (en) * | 2019-12-30 | 2020-04-17 | 大连理工大学 | Method for rapidly and efficiently detecting contents of multiple antibiotics in vegetables simultaneously |
| CN112444591A (en) * | 2019-08-30 | 2021-03-05 | 谱尼测试集团上海有限公司 | Liquid chromatography-tandem mass spectrometry method for determining residual quantity of ametoctradin in plant food |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102197819A (en) * | 2011-04-06 | 2011-09-28 | 江苏宝灵化工股份有限公司 | Bactericidal composition and its application |
| CN102696637B (en) * | 2012-04-19 | 2013-11-06 | 云南省农业科学院生物技术与种质资源研究所 | Gentiopicroside pharmaceutical preparation and application thereof in prevention and treatment tobacco mosaic virus (TMV) disease |
| US20130324493A1 (en) * | 2012-06-01 | 2013-12-05 | North Carolina State University | Compositions comprising ningnanmycin and uses therefor |
| CN103858885A (en) * | 2014-04-11 | 2014-06-18 | 山东省烟台市农业科学研究院 | Bactericidal composition for controlling apple diseases and application thereof |
| CN104497000A (en) * | 2014-12-15 | 2015-04-08 | 云南中烟工业有限责任公司 | Tobacco mosaic virus-resistant plant flavonoids compound as well as preparation method and applications thereof |
| WO2015160619A1 (en) * | 2014-04-16 | 2015-10-22 | Bayer Cropscience Lp | Compositions comprising ningnanmycin and a fungicide |
-
2016
- 2016-06-06 CN CN201610404473.7A patent/CN107462652B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102197819A (en) * | 2011-04-06 | 2011-09-28 | 江苏宝灵化工股份有限公司 | Bactericidal composition and its application |
| CN102696637B (en) * | 2012-04-19 | 2013-11-06 | 云南省农业科学院生物技术与种质资源研究所 | Gentiopicroside pharmaceutical preparation and application thereof in prevention and treatment tobacco mosaic virus (TMV) disease |
| US20130324493A1 (en) * | 2012-06-01 | 2013-12-05 | North Carolina State University | Compositions comprising ningnanmycin and uses therefor |
| CN103858885A (en) * | 2014-04-11 | 2014-06-18 | 山东省烟台市农业科学研究院 | Bactericidal composition for controlling apple diseases and application thereof |
| WO2015160619A1 (en) * | 2014-04-16 | 2015-10-22 | Bayer Cropscience Lp | Compositions comprising ningnanmycin and a fungicide |
| CN104497000A (en) * | 2014-12-15 | 2015-04-08 | 云南中烟工业有限责任公司 | Tobacco mosaic virus-resistant plant flavonoids compound as well as preparation method and applications thereof |
Non-Patent Citations (4)
| Title |
|---|
| TIELONG WANG 等: "Dissipation and Residue Determination of Ningnanmycin in Cucumber and Soil by High Performance Liquid Chromatography with Ultraviolet Detector", 《BULLETIN ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY》 * |
| 向固西 等: "一种新的农用抗生素——宁南霉素", 《微生物学报》 * |
| 张婷 等: "农用抗生素XBP-03-A的分离及结构鉴定", 《湖南农业科学》 * |
| 王芳 等: "宁南霉素液相检测条件的确定", 《粮油科技》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108562673A (en) * | 2018-07-17 | 2018-09-21 | 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 spectrum detection method measuring Ningnanmycin content in tomato |
| CN110261509A (en) * | 2019-07-10 | 2019-09-20 | 中山永恒检测科技有限公司 | The high-efficiency liquid chromatography method for detecting of Ningnanmycin residual quantity in a kind of measurement rice |
| CN110261511A (en) * | 2019-07-16 | 2019-09-20 | 中山永恒检测科技有限公司 | The Liquid Chromatography-Tandem Mass Spectrometry detection method of Ningnanmycin residual quantity in a kind of cucumber |
| CN112444591A (en) * | 2019-08-30 | 2021-03-05 | 谱尼测试集团上海有限公司 | Liquid chromatography-tandem mass spectrometry method for determining residual quantity of ametoctradin in plant food |
| CN112444591B (en) * | 2019-08-30 | 2024-01-30 | 谱尼测试集团上海有限公司 | Liquid chromatography tandem mass spectrometry for determining residual quantity of flumetsulam in vegetable food |
| CN111024854A (en) * | 2019-12-30 | 2020-04-17 | 大连理工大学 | Method for rapidly and efficiently detecting contents of multiple antibiotics in vegetables simultaneously |
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