NL2033320B1 - Method for detecting cmpf content in plasma by high performance liquid chromatography tandem mass spectrometry - Google Patents
Method for detecting cmpf content in plasma by high performance liquid chromatography tandem mass spectrometry Download PDFInfo
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- NL2033320B1 NL2033320B1 NL2033320A NL2033320A NL2033320B1 NL 2033320 B1 NL2033320 B1 NL 2033320B1 NL 2033320 A NL2033320 A NL 2033320A NL 2033320 A NL2033320 A NL 2033320A NL 2033320 B1 NL2033320 B1 NL 2033320B1
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 23
- 238000004885 tandem mass spectrometry Methods 0.000 title claims abstract description 17
- WMCQWXZMVIETAO-UHFFFAOYSA-N 2-(2-carboxyethyl)-4-methyl-5-propylfuran-3-carboxylic acid Chemical compound CCCC=1OC(CCC(O)=O)=C(C(O)=O)C=1C WMCQWXZMVIETAO-UHFFFAOYSA-N 0.000 claims abstract description 84
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 238000002203 pretreatment Methods 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 8
- 238000011002 quantification Methods 0.000 claims abstract description 8
- 238000011088 calibration curve Methods 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 239000000126 substance Substances 0.000 claims description 23
- 239000003960 organic solvent Substances 0.000 claims description 14
- 150000002500 ions Chemical class 0.000 claims description 13
- 238000002552 multiple reaction monitoring Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000004807 desolvation Methods 0.000 claims description 8
- 230000006920 protein precipitation Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- IWXRPVHRDWXIEA-UHFFFAOYSA-N azanium formate hydrate Chemical compound [NH4+].O.[O-]C=O IWXRPVHRDWXIEA-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 238000004704 ultra performance liquid chromatography Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 102000007562 Serum Albumin Human genes 0.000 claims description 2
- 108010071390 Serum Albumin Proteins 0.000 claims description 2
- 244000309464 bull Species 0.000 claims description 2
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 238000010813 internal standard method Methods 0.000 abstract description 3
- 238000004587 chromatography analysis Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 44
- 238000003018 immunoassay Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 238000010811 Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry Methods 0.000 description 5
- 208000002705 Glucose Intolerance Diseases 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 4
- 241001669573 Galeorhinus galeus Species 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 210000003719 b-lymphocyte Anatomy 0.000 description 3
- 206010012601 diabetes mellitus Diseases 0.000 description 3
- 208000004104 gestational diabetes Diseases 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 201000009104 prediabetes syndrome Diseases 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 230000003914 insulin secretion Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 206010018429 Glucose tolerance impaired Diseases 0.000 description 1
- 101001091385 Homo sapiens Kallikrein-6 Proteins 0.000 description 1
- 102100034866 Kallikrein-6 Human genes 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 230000023852 carbohydrate metabolic process Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004129 fatty acid metabolism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 210000000496 pancreas Anatomy 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008844 regulatory mechanism Effects 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002441 uremic toxin Substances 0.000 description 1
- 238000003260 vortexing Methods 0.000 description 1
Classifications
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
-
- 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
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Claims (3)
1. Werkwijze voor het detecteren van het gehalte aan 3-carboxy-4- methyl-5-propyl-2-furanpropaanzuur (CMPF) in plasma door middel van tandemmassaspectrometrie met hoogwaardige vloeistofchromato- grafie, met het kenmerk, dat de werkwijze de volgende stappen om- vat: voorbehandeling van plasmamonster: nauwkeurig pipetteren van 100 uL van een plasmamonster en plaatsen op een 96-wells eiwitprecipi- tatieplaat, toevoegen van een organisch oplosmiddel met een inter- ne standaard van CMPF-isotoop, plaatsen in een oscillator met con- stante temperatuur, schudden bij 700 rpm gedurende 3 min, plaatsen op een apparaat met positieve druk, aanpassen van een stroomsnel- heid tot 40 psi, het nemen van gefilterde oplossing en het gebrui- ken als een detectiemonster voor tandemmassaspectrometrie voor vloeistofchromatografie voor stand-by; en detectie van het CMPF-gehalte in het voorbehandelde plasmamonster met behulp van de tandemmassaspectrometrie met hoogwaardige vloei- stofchromatografie: eerst met behulp van hoogwaardige vloeistof- chromatografie om CMPF te scheiden, en vervolgens met behulp van een interne standaardmethode voor massaspectrometrie voor kwanti- ficering, met behulp van de concentratie verhouding van een CMPF- doelverbinding en een interne CMPF-isotoopstandaard als X-as, en met behulp van de piekoppervlakverhouding van de CMPF- doelverbinding en de interne CMPF-isotoopstandaard als Y-as, om een kalibratiecurve vast te stellen, en het berekenen van het CMPF-gehalte in het plasma, waarbij de specifieke instrument- omstandigheden als volgt zijn: (1) omstandigheden voor hoogwaardige vloeistofchromatografie: mobiele fase A: 5 mM ammoniumformiaat water; mobiele fase B: 0,1% mierenzuur + methanol; chromatografisch kolommodel: Waters UPLC HSS C18SB 2,1 mmx50 mm, 1,8 um de kolomtemperatuur is 40 °C + 5 °C, het injectievolume is 10 pL, de temperatuur van een monsterinjectielade is 10 °C + 5 °C, en de stroomsnelheid is 0,4 ml / min; en er wordt een gradiëntelutiemodus gebruikt, zoals weergegeven in tabel 1 hieronder: Tabel 1: Gradiënt elutie procedure Tijd (min) Stroomsnelheid (mL/min) A% B% Curve 00 0400 800 200 6
0.5 0.400 80.0 200 6
0.8 0.400 950 50 6 15 0.400 950 50 6 1,51 0.400 80.0 200 6
2.0 0.400 800 200 6 (2) massaspectrometrie omstandigheden: ionisatiemodus: in een elektrospray-positieve ionen modus wordt een massaspectrumscanmodus van meervoudige reactiebewaking (MRM) gebruikt, de capillaire spanning is 4,0 kV; de temperatuur van de ionenbron is 150 °C; de desolvatie gastemperatuur is 650 °C; het desolvatiegasdebiet is 650 l/u; en de doelverbinding en de interne standaard van de isotoop worden gelijktijdig ge- volgd; en MRM-modus: ionparameter: CMPF: 239.1596>151.114, de kegelspan- ning is 32 V, en de botsingsenergie is 16 V; en CMPF-d3:
242.1596>154.173, de kegelspanning is 32 V en de botsingsenergie is 18 V.
2. Werkwijze voor het detecteren van het CMPF-gehalte in het plas- ma door middel van tandemmassaspectrometrie met hoogwaardige vloeistofchromatografie volgens conclusie 1, met het kenmerk, dat bij de voorbehandeling van het plasmamonster het toegevoegde orga- nische oplosmiddel dat de interne standaard van het CMPF-isotoop bevat, wordt bereid volgens de volgende werkwijze: gebruik de me- thanol als oplosmiddel om 1 mg/ml CMPF-d3 standaardstof- voorraadoplossing te bereiden en gebruik vervolgens de methanol om het organische oplosmiddel te bereiden dat 1,0 pg/ml CMPF-d3 be-
vat.
3. Werkwijze voor het detecteren van het CMPF-gehalte in het plas- ma door middel van tandemmassaspectrometrie met hoogwaardige vloeistofchromatografie volgens conclusie 1, met het kenmerk, dat de CMPF-doelverbinding wordt bereid door de volgende werkwijze: met gebruikmaking van de methanol als oplosmiddel om 1 mg/ml CMPF- standaardstofvoorraadoplossing te bereiden, en vervolgens gebruik maken van 5% m/v stierserumalbumine (BSA) -oplossing om in totaal 7 gradiënten van gemengde standaardstofoplossing te bereiden met CMPF-concentraties van 0,02 pg/ml, 0,1 ug/ml , 0,5 pg/ml, 1,0 pg/mL, 5,0 pg/ml, 10,0 pg/mL, en 50 pg/ml en het afzonderlijk in een bruine fles van 1,5 ml brengen en bij -20 °C bewaren voor la- ter gebruik.
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CN104822378A (zh) * | 2012-09-21 | 2015-08-05 | 多伦多大学理事会 | 作为糖尿病的生物标志物的cmpf和相关方法 |
CN109884317B (zh) * | 2019-03-12 | 2022-03-08 | 杭州博谱医药科技有限公司 | 氧化型硫代辅酶i在均相酶免疫诊断试剂中的应用 |
CN110907569A (zh) * | 2019-12-25 | 2020-03-24 | 山东英盛生物技术有限公司 | 一种同时检测血液样品中4种蛋白结合尿毒症毒素的方法 |
CN112326829A (zh) * | 2020-11-03 | 2021-02-05 | 浙江大学滨海产业技术研究院 | 一种基于代谢组学通路的慢性肾病早期预警方法 |
CN114152743A (zh) * | 2021-12-02 | 2022-03-08 | 沈阳易康元血液透析科技有限公司 | 一种检测cmpf的化学发光免疫检测试剂盒及其检测方法 |
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Non-Patent Citations (4)
Title |
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MARIA A. LANKINEN ET AL: "CMPF Does Not Associate with Impaired Glucose Metabolism in Individuals with Features of Metabolic Syndrome", PLOS ONE, vol. 10, no. 4, 15 April 2015 (2015-04-15), pages e0124379, XP055438452, DOI: 10.1371/journal.pone.0124379 * |
NIWA T ET AL: "Rapid assay for furancarboxylic acid accumulated in uremic serum using high-performance liquid chromatography and on-line mass spectrometry", CLINICA CHIMICA ACTA, ELSEVIER BV, AMSTERDAM, NL, vol. 226, no. 1, 1 April 1994 (1994-04-01), pages 89 - 94, XP024785526, ISSN: 0009-8981, [retrieved on 19940401], DOI: 10.1016/0009-8981(94)90106-6 * |
SUZUKI YOSUKE ET AL: "Simultaneous quantification of coproporphyrin-I and 3-carboxy-4-methyl-5-propyl-2-furanpropanoic acid in human plasma using ultra-high performance liquid chromatography coupled to tandem mass spectrometry", JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, ELSEVIER B.V, AMSTERDAM, NL, vol. 184, 24 February 2020 (2020-02-24), XP086128274, ISSN: 0731-7085, [retrieved on 20200224], DOI: 10.1016/J.JPBA.2020.113202 * |
YOSHIHARU ITOH ET AL: "Protein-bound uremic toxins in hemodialysis patients measured by liquid chromatography/tandem mass spectrometry and their effects on endothelial ROS production", ANALYTICAL AND BIOANALYTICAL CHEMISTRY, SPRINGER, BERLIN, DE, vol. 403, no. 7, 25 March 2012 (2012-03-25), pages 1841 - 1850, XP035059651, ISSN: 1618-2650, DOI: 10.1007/S00216-012-5929-3 * |
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