CN109030637A - The detection method of triethylphosphine acid Aluminium residual in a kind of food - Google Patents
The detection method of triethylphosphine acid Aluminium residual in a kind of food Download PDFInfo
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- CN109030637A CN109030637A CN201710425101.7A CN201710425101A CN109030637A CN 109030637 A CN109030637 A CN 109030637A CN 201710425101 A CN201710425101 A CN 201710425101A CN 109030637 A CN109030637 A CN 109030637A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of detection methods of triethylphosphine acid Aluminium residual in food, sample is with the extraction with aqueous solution of 50% acetonitrile, after being centrifuged, supernatant is through C18-SPE Solid Phase Extraction column purification, remove impurity, utilizing hydrophilic Interaction Chromatography HILIC chromatography post separation, it connects triple level four bars mass spectrums (UPLC/MS/MS), multiple-reaction monitoring scan pattern (MRM), quantified by external standard method, the method detection limit of phosethyl-Al of the present invention is 0.01mg/kg, 0.01mg/kg to 0.1mg/kg concentration level average recovery rate 71% ~ 95%, relative standard deviation RSD≤10%.Method of the invention is easy to operate, favorable reproducibility, effectively removes the impurity in sample extracting solution, quickly can carry out qualitative and quantitative analysis simultaneously to phosethyl-Al pesticide in food.
Description
Technical field
The invention belongs to a kind of inspections of triethylphosphine acid Aluminium residual in food detection method technical field more particularly to food
Survey method.
Background technique
Three second aluminum phosphates (Fosetyl-aluminium) are a kind of organic phosphates systemic fungicides, have protection and control
Treatment effect.Because of it to phycomycetes such as Peronospora, Phytophthoras caused by disease have good preventive effect, so being widely used in vegetable
In the plantation of dish.Three second aluminum phosphates in gas chromatographic flame photometric detector detection vegetables are mostly used at present, as Japan improves people's living condition labor
Dynamic to save the official method announced, this method uses gas phase color after needing to be derivatized to volatile compound with diazomethane again
Spectrum detection.Diazomethane toxicity is big, is not easy to store, and prepares the danger for the explosion that happens occasionally.Be not suitable in this way conventional
The detection of gross sample in testing laboratory.Three second aluminum phosphates have high water solubility, and the ethyl connected in molecule makes it again
Property with organic molecule, this characteristic determine that three second aluminum phosphates can be analyzed by high performance liquid chromatography tandem mass spectrum.State
It is inside and outside to have been reported that with three second phosphoric acid Aluminium residuals in high performance liquid chromatography tandem mass spectrometry measurement lettuce, hops and waste water, but
These methods are relatively complicated, and reagent consumption is big, unfriendly to environment, and batch processing is poor, and it is more multiple not to be suitable for matrix
Miscellaneous greenery vegetables, oil-containing based food.Currently, China there is no the national standard of the detection method of phosethyl-Al in food.Cause
This, quick, effective, sensitive, the reliable and practical residue analysis method of foundation there is important reality to anticipate food safety
Justice.
Summary of the invention
The present invention in view of the above-mentioned deficiencies in the prior art, using liquid-liquid extraction techniques and solid phase extraction techniques to sample
Product are pre-processed, and knot and hydrophilic interaction HILIC chromatographic separation technology, high performance liquid chromatography tandem mass spectrum technology provide one kind
Fast and efficiently in food the detection of triethylphosphine acid Aluminium residual method.
The technical scheme to solve the above technical problems is that in food the detection of triethylphosphine acid Aluminium residual method,
The following steps are included:
(1) extract: weigh sample into plastic centrifuge tube, be added 50% acetonitrile aqueous solution, sufficient vortex mix, carry out from
The heart；
(2) it purifies: the aqueous solution obtained after step (1) centrifugation is crossed into C18 Solid Phase Extraction column purification；
(3) it crosses film filtering: the scavenging solution that step (2) obtains being crossed into film, to upper machine testing；
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: contain 0.2% formic acid 5mM formic acid aqueous ammonium+acetonitrile (100+5, V/V), B: acetonitrile
Ionization mode: ESI- mode
Chromatographic column: ACQUITY UPLCTMBEH Amide Column (2.1 mm of internal diameter × 150 mm of length, partial size 1.8
μm)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Mass Spectrometry Conditions: multiple-reaction monitoring (MRM) scan pattern, phosethyl-Al multiple-reaction monitoring (MRM) sweep parameter are as follows:
Wherein band * is quota ion.
Further, as described in step (1) extract is to weigh 10.0 g of sample of uniform sample preparation in 50 mL centrifuge tubes,
The aqueous solution of 20 mL, 50% acetonitrile is added, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, and supernatant is transferred to one
In 50 mL colorimetric cylinders, residue uses the extraction with aqueous solution of 20 mL, 50% acetonitrile again, and sufficient vortex mixes, 4000 r/min from
5 min of the heart merges extracting solution twice, and is settled to 50 mL with acetonitrile, to be clean after mixing.Described in step (2)
Purification is that 5.0 mL of extracting solution that step (1) obtains is crossed C18-SPE solid-phase extraction column, and purification is directly collected, solid phase extraction
Column is taken successively to be activated in advance with the extracting solution of 3 mL acetonitriles, 3 mL water, 3 mL steps (1).Film mistake is crossed described in step (3)
The scavenging solution that step (2) obtains is crossed 0.22 μm of teflon membrane filter (PTFE filter membrane) by filter formula, is filtered in sample injection bottle.Step
(4) the UPLC/MS/MS detection described in is step (3) resulting filtrate, according to instrument condition described in step (4), upper machine examination
It surveys.
The beneficial effects of the present invention are: the method pair that the present invention is combined using liquid-liquid extraction techniques and solid phase extraction techniques
Sample is pre-processed.Liquid-liquid extraction techniques basic operation is to utilize compound in the solvent of two kinds immiscible (or slightly soluble)
The difference of solubility or distribution coefficient is transferred to compound in another solvent from a kind of solvent；Solid phase extraction techniques
Basic operation is exactly that the target compound or impurity absorption in fluid sample are made the matrix of sample and done using solid absorbent
It disturbs compound to separate with target compound, achievees the purpose that separation and enrichment target compound.The present invention utilizes hydrophilic interaction
HILIC chromatographic separation technology carries out chromatographic isolation to sample.Hydrophilic interaction HILIC chromatographic isolation is to be different from normal-phase chromatography, anti-
A kind of anti-reversed phase chromatography separation technology of phase chromatography and ion chromatography, it can retain and separate highly polar phosethyl-Al.Three second
More reaction detections (MRM) spectrogram of phosphonic acids aluminium is detailed in Fig. 1.The method of the present invention detects phosethyl-Al in food, can be quick
Carry out qualitative, quantitative, detection limit is fully able to meet detection demand, and detection efficiency greatly promotes.
The present invention is extracted using 50% acetonitrile solution, is then passed through C18-SPE Solid Phase Extraction column purification, can effectively be gone
Except fatty acid, sugar, the fat etc. in component interfere impurity, avoid in conventional method using toxic, dangerous examinations such as diazomethanes
Agent, the present invention are very friendly to human and environment.
The present invention is to be detected after sample dilutes sample introduction using highly sensitive UPLC-MS/MS, chromatography can be completed within 7 minutes
Separation and sample introduction, external standard method can be qualitative, quantitative.It is compared with the traditional method compared with the present invention does not need the rotation in conventional method
The cumbersome enrichment procedures such as evaporation, the dry, concentration of nitrogen, do not need 30 minutes or even longer color of efficient liquid-phase chromatography method
Spectrum separation and sample injection time, the invention saves time and labor cost-saving, and efficiently, quickly, it is accurate.
Detailed description of the invention
Fig. 1 is phosethyl-Al multiple-reaction monitoring (MRM) spectrogram.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Phosethyl-Al standard solution is prepared, negative spinach, apple, rice, pork are taken, homogeneous crushes uniformly, respectively
The mixed mark of 3 kinds of various concentrations is added into spinach, apple, rice, pork, addition concentration is 10 μ g/kg, 20 μ g/kg, 100 μ
G/kg, freezer storage is spare in -18 DEG C of refrigerators, pitch-based sphere be equal to or less than China limit standard, each content
Level is repeated 10 times.
Embodiment 1: taking above-mentioned spinach samples, detects its phosethyl-Al residual content, steps are as follows:
(1) it extracts: weighing 10.0 g spinach samples into 50 mL plastic centrifuge tubes, the aqueous solution of 20 mL, 50% acetonitrile is added
, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, and supernatant is transferred in a 50 mL colorimetric cylinders, and residue uses 20 again
The extraction with aqueous solution of 50% acetonitrile of mL, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, merge extracting solution twice, are used in combination
Acetonitrile is settled to 50 mL, to be clean after mixing.；
(2) it purifies: 5.0 mL of extracting solution obtained after step (1) centrifugation being crossed into C18-SPE solid-phase extraction column, purifies, directly receives
Collection, the solid-phase extraction column are successively activated with the extracting solution of 3 mL acetonitriles, 3 mL water, 3 mL steps (1) in advance；
(3) cross film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane), filter into
In sample bottle, to upper machine testing；
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: contain 0.2% formic acid 5mM formic acid aqueous ammonium+acetonitrile (100+5, V/V), B: acetonitrile
Ionization mode: ESI- mode
Chromatographic column: ACQUITY UPLCTMBEH Amide Column (2.1 mm of internal diameter × 150 mm of length, partial size 1.8
μm)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Phosethyl-Al multiple-reaction monitoring (MRM) sweep parameter is as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of phosethyl-Al residual content in obtained spinach are shown in Table 1.
Embodiment 2: taking above-mentioned apple sample, detects its phosethyl-Al residual content, steps are as follows:
(1) it extracts: weighing 10.0 g apple samples into 50 mL plastic centrifuge tubes, the aqueous solution of 20 mL, 50% acetonitrile is added
, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, and supernatant is transferred in a 50 mL colorimetric cylinders, and residue uses 20 again
The extraction with aqueous solution of 50% acetonitrile of mL, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, merge extracting solution twice, are used in combination
Acetonitrile is settled to 50 mL, to be clean after mixing.；
(2) it purifies: 5.0 mL of extracting solution obtained after step (1) centrifugation being crossed into C18-SPE solid-phase extraction column, purifies, directly receives
Collection, the solid-phase extraction column are successively activated with the extracting solution of 3 mL acetonitriles, 3 mL water, 3 mL steps (1) in advance；
(3) cross film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane), filter into
In sample bottle, to upper machine testing；
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: contain 0.2% formic acid 5mM formic acid aqueous ammonium+acetonitrile (100+5, V/V), B: acetonitrile
Ionization mode: ESI- mode
Chromatographic column: ACQUITY UPLCTMBEH Amide Column (2.1 mm of internal diameter × 150 mm of length, partial size 1.8
μm)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
Phosethyl-Al multiple-reaction monitoring (MRM) sweep parameter is as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of phosethyl-Al residual content in obtained apple are shown in Table 1.
Embodiment 3: taking above-mentioned rice sample, detects its phosethyl-Al residual content, steps are as follows:
(1) it extracts: weighing 10.0 g rice samples into 50 mL plastic centrifuge tubes, the aqueous solution of 20 mL, 50% acetonitrile is added
, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, and supernatant is transferred in a 50 mL colorimetric cylinders, and residue uses 20 again
The extraction with aqueous solution of 50% acetonitrile of mL, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, merge extracting solution twice, are used in combination
Acetonitrile is settled to 50 mL, to be clean after mixing.；
(2) it purifies: 5.0 mL of extracting solution obtained after step (1) centrifugation being crossed into C18-SPE solid-phase extraction column, purifies, directly receives
Collection, the solid-phase extraction column are successively activated with the extracting solution of 3 mL acetonitriles, 3 mL water, 3 mL steps (1) in advance；
(3) cross film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane), filter into
In sample bottle, to upper machine testing；
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: contain 0.2% formic acid 5mM formic acid aqueous ammonium+acetonitrile (100+5, V/V), B: acetonitrile
Ionization mode: ESI- mode
Chromatographic column: ACQUITY UPLCTMBEH Amide Column (2.1 mm of internal diameter × 150 mm of length, partial size 1.8
μm)
Sample volume: 1 μ L
Chromatographic isolation item:
Phosethyl-Al multiple-reaction monitoring (MRM) sweep parameter is as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of phosethyl-Al residual content in obtained rice are shown in Table 1.
Embodiment 4: taking above-mentioned pork sample, detects its phosethyl-Al residual content, steps are as follows:
(1) it extracts: weighing 10.0 g pork samples into 50 mL plastic centrifuge tubes, the aqueous solution of 20 mL, 50% acetonitrile is added
, sufficient vortex mixes, and 4000 r/min are centrifuged 5 min, and supernatant is transferred in a 50 mL colorimetric cylinders, and residue uses 20 again
The extraction with aqueous solution of 50% acetonitrile of mL, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, merge extracting solution twice, are used in combination
Acetonitrile is settled to 50 mL, to be clean after mixing.；
(2) it purifies: 5.0 mL of extracting solution obtained after step (1) centrifugation being crossed into C18-SPE solid-phase extraction column, purifies, directly receives
Collection, the solid-phase extraction column are successively activated with the extracting solution of 3 mL acetonitriles, 3 mL water, 3 mL steps (1) in advance；
(3) cross film filtering: the scavenging solution that step (2) obtains is crossed into 0.22 μm of teflon membrane filter (PTFE filter membrane), filter into
In sample bottle, to upper machine testing；
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: contain 0.2% formic acid 5mM formic acid aqueous ammonium+acetonitrile (100+5, V/V), B: acetonitrile
Ionization mode: ESI- mode
Chromatographic column: ACQUITY UPLCTMBEH Amide Column (2.1 mm of internal diameter × 150 mm of length, partial size 1.8
μm)
Sample volume: 1 μ L
Chromatographic separation condition:
Phosethyl-Al multiple-reaction monitoring (MRM) sweep parameter is as follows:
Band * is quota ion in table.
The average recovery rate and relative standard deviation RSD of phosethyl-Al residual content in obtained pork are shown in Table 1.
Triethylphosphine acid aluminium recovery and relative standard deviation (n=10) in 1 food of table
For the average recovery rate of phosethyl-Al 71% ~ 95%, relative standard is inclined in various food it can be seen from data in table 1
Poor RSD≤10%, the rate of recovery and relative standard deviation meet Detecting Pesticide standard.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. the detection method of triethylphosphine acid Aluminium residual in a kind of food, it is characterised in that the following steps are included:
(1) it extracts: weighing sample into plastic centrifuge tube, the aqueous solution of 50% acetonitrile is added, sufficient vortex is mixed, is centrifuged,
Obtain extracting solution；
(2) it purifies: the extracting solution obtained after step (1) centrifugation being crossed into C18 Solid Phase Extraction column purification, is purified liquid；
(3) it crosses film filtering: the scavenging solution that step (2) obtains being crossed into film, to upper machine testing；
(4) UPLC/MS/MS is detected:
Instrument condition:
Mobile phase: A: contain 0.2% formic acid 5mM formic acid aqueous ammonium+acetonitrile (100+5, V/V), B: acetonitrile
Ionization mode: ESI- mode
Chromatographic column: ACQUITY UPLCTMBEH Amide Column (internal diameter 2.1mm × 150 mm of length, 1.8 μm of partial size)
Sample volume: 1 μ L
Chromatographic separation condition is as follows:
；
Mass Spectrometry Conditions: multiple-reaction monitoring (MRM) scan pattern, phosethyl-Al multiple-reaction monitoring (MRM) sweep parameter are as follows:
,
Wherein band * is quota ion.
2. the detection method of triethylphosphine acid Aluminium residual in food according to claim 1, it is characterised in that in step (1)
The extraction is to weigh 10.0 g of sample of uniform sample preparation in 50 mL centrifuge tubes, and the water-soluble of 20 mL, 50% acetonitrile is added
Liquid, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, and supernatant is transferred in a 50 mL colorimetric cylinders, and residue is used again
The extraction with aqueous solution of 20 mL, 50% acetonitrile, sufficient vortex mix, and 4000 r/min are centrifuged 5 min, merge extracting solution twice,
And 50 mL are settled to acetonitrile, it is to be clean after mixing.
3. the detection method of triethylphosphine acid Aluminium residual in food according to claim 1, it is characterised in that in step (2)
The purification is that 5.0 mL of extracting solution that step (1) obtains is crossed C18-SPE solid-phase extraction column, and purification is directly collected, should
Solid-phase extraction column is successively activated with the extracting solution of 3 mL acetonitriles, 3 mL water, 3 mL steps (1) in advance.
4. the detection method of triethylphosphine acid Aluminium residual in middle food according to claim 1, it is characterised in that step (3)
Described in cross film filtering be that the scavenging solution for obtaining step (2) is crossed 0.22 μm of teflon membrane filter (PTFE filter membrane), filter
Enter in sample injection bottle, to upper machine testing.
5. the detection method of triethylphosphine acid Aluminium residual in food according to claim 1, it is characterised in that in step (4)
The UPLC/MS/MS detection is step (3) resulting filtrate, according to instrument condition described in step (4), upper machine testing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110824090A (en) * | 2019-11-27 | 2020-02-21 | 日照健安检测技术服务有限公司 | Method for rapidly detecting residual quantity of fosetyl-aluminum in vegetables |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1684068A1 (en) * | 2005-01-25 | 2006-07-26 | Bayer CropScience S.A. | Analysis method for pesticide compounds |
| CN101650344A (en) * | 2009-08-02 | 2010-02-17 | 青岛科技大学 | Detection and analysis method of content of fosetyl-aluminium |
| CN102944621A (en) * | 2012-11-12 | 2013-02-27 | 深圳市谱尼测试科技有限公司 | Method for determining residual quantity of fosetyl-aluminium in environmental sample |
| CN106645539A (en) * | 2017-03-10 | 2017-05-10 | 中国热带农业科学院分析测试中心 | Method for detecting phosethyl-aluminum through ultra-high performance liquid chromatography-tandem mass spectrometry |
-
2017
- 2017-06-08 CN CN201710425101.7A patent/CN109030637A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1684068A1 (en) * | 2005-01-25 | 2006-07-26 | Bayer CropScience S.A. | Analysis method for pesticide compounds |
| CN101107517A (en) * | 2005-01-25 | 2008-01-16 | 拜尔农科股份有限公司 | Method of analyzing phosphorous acid, fosetyl-al or both simultaneously |
| CN101650344A (en) * | 2009-08-02 | 2010-02-17 | 青岛科技大学 | Detection and analysis method of content of fosetyl-aluminium |
| CN102944621A (en) * | 2012-11-12 | 2013-02-27 | 深圳市谱尼测试科技有限公司 | Method for determining residual quantity of fosetyl-aluminium in environmental sample |
| CN106645539A (en) * | 2017-03-10 | 2017-05-10 | 中国热带农业科学院分析测试中心 | Method for detecting phosethyl-aluminum through ultra-high performance liquid chromatography-tandem mass spectrometry |
Non-Patent Citations (4)
| Title |
|---|
| JAN POUSTKA 等: "Potential of Liquid Chromatography–Atmospheric Pressure Chemical Ionisation Tandem Mass Spectrometry for Determination of Fosetyl-aluminium Residues in Dried Hops", 《CZECH J. FOOD SCI.》 * |
| ROCÍONORTES-MÉNDEZ 等: "Determination of polar pesticides in olive oil and olives by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry and high resolution mass spectrometry", 《TALANTA》 * |
| 王洪艳 等: "高效液相色谱串联质谱法检测菠菜中三乙磷酸铝残留量", 《农产品加工·学刊》 * |
| 范志先 等: "离子对反相高效液相色谱-蒸发光散射检测法测定三乙膦酸铝的含量", 《色谱》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110824090A (en) * | 2019-11-27 | 2020-02-21 | 日照健安检测技术服务有限公司 | Method for rapidly detecting residual quantity of fosetyl-aluminum in vegetables |
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Application publication date: 20181218 |