Potential sources of contamination on Mass Spectrometers and suggested cleaning procedures
|
|
- Anna Dalton
- 5 years ago
- Views:
Transcription
1 Potential sources of contamination on Mass Spectrometers and suggested cleaning procedures Purpose: This document provides information on potential sources of background contamination commonly encountered on mass spectrometers, which can degrade the quality of results by increasing the background, reducing sensitivity. 1. Possible background ions Name: Polyethylene glycol (PEG). Mass spectrum: Usually seen in ESI + as a series of ions separated by 44Da. Sources: 1) Organic solvents e.g. methanol, water, acetonitrile, isopropanol. 2) Dermatological creams 3) Plastic gloves, protein extraction detergents (e.g. Triton X100, X114), 4) Glassware detergents 5) Cutting solutions 6) MS calibration solutions 7) Column manufacture _50ACN_L02_B1 120 (2.284) Cm (120:140) : TOF MS ES+ 176 PEG-LIKE CONTAMINATION 50:50 ACN:H2O +0.1% formic acid Combined 21 spectra % m/z Figure 1: Typical PEG contamination 34301_1 1 of 9
2 Name: Phthalates Mass Spectrum: Seen as [M+H] + in ESI + at m/z = 391, 419 and 447. Generally attributed to Di-isooctylphthalate, Dinonylphthalate, Diisodecyl phthalate respectively. Can form adduct ions with sodium, potassium and ammonium ions. e.g. for Di-isooctylphthalate [M+Na] + = 413, [M+K] + = 429, [2M+NH 4 ] + = 798, [2M+Na] + = 803, depending on conditions. Sources: 1) Can be extracted from plastics e.g.. Tubing, plastic bottles, plastic vials, vial caps. 2) Can be airborne and enter solvents by absorption. Notes: A wide range of phthalate compounds are used as plasticizers in many common plastics. Ion signals arising from these species can be more intense when utilising high aqueous conditions due to increased solubility. Figure 2: Typical pthalate background ions Name: Metal ions (e.g.. Na +,K +,Fe 2/3+,Cu 2+, Pt + ) Mass Spectrum: Cause adduct formation e.g.. [M+Na] +, [M+K + ], etc. Fe 3+ can form adducts with varying numbers of acetates from acetic acid or acetate buffers to give characteristic ESI+ ions at m/z = and Sources: 1) Solvents 2) Buffers 3) Additives (e.g. acetic/formic acid) 4) Metal components 34301_1 2 of 9
3 Notes: Solvent manufacturers usually state trace metal content of their solvents on the side of the bottle, or on the MSDS sheet. These can vary a great deal between manufacturer and also the particular grade of solvent. E.g. HPLC grade usually has a lower metal content than other grades. Name: Siloxanes e.g.. Polydimethylcyclicsiloxanes of monomeric unit (Si(CH 3 ) 2 O) n Mass Spectrum: Observed at m/z = 445, 519, 593, 667, 741. Generally can be attributed to decamethylsiloxane, dodecamethylsiloxane, tetradecamethylsiloxane, hexadecamethylsiloxane, octacdecamethylsiloxane respectively. Additional masses can be observed at m/z = 429 and 503. Also seen are ammonium adducts (+17Da) and ions as a results of a methyl group loss. Sources: 1) Silica capillary, HPLC column packing materials etc 2) Ubiquitous airborne contaminants Notes: Generally seen more often under NanoFlow conditions. Procedures for removal of these background ions are limited due to the overwhelming presence in the atmosphere. Detuning the probe positions can reduce background ions while not severely reducing sample signal. A higher concentration of nitrogen in the source region can also reduce siloxane production at the probe tip. The paper: Schlosser A, Volkmer-Engert R, J. Mass Spectrom, 2003, 38, p is a good reference for these ions. Figure 3: Typical siloxane background ions on a Nanospray source _1 3 of 9
4 2. Minimizing background ions a) Solvents and additives Use the highest purity solvents HPLC grade or better i. Solvents 1. The current solvents in use at Waters MS Technologies Atlas Park are Water (Fisher W/0106/17) Methanol (Fisher M/4058/17) and Acetonitrile (Sigma 34888). 2. Some HPLC grade solvents contain PEG. PEG is not seen by a UV detector, but will be observed using an MS. Always read the label. 3.Some HPLC grade solvents contain metal ions. 4. Fresh solvents are better than previously opened bottles. 5. Additives should also be pure. 90% formic acid solution contains 10% other compounds! Analytical grade (>99%) is recommended. ii. Water can be a major source of contamination 1. On-line water systems (Milli-Q) must be maintained. 18 MOhm water is not free of organic contamination. Organic filters and UV lights increase the purity for HPLC use. 2. Bottled water may not be any better than water from Milli-Q. After a bottle has been opened, it will accumulate contaminates by absorption from the air, through any secondary container, or via general use (e.g.. pipettes etc). Storage of water in plastic containers is NOT recommended. Water can be further purified by passing it through a clean C18 column to trap organic materials. This can be done on-line in a high-pressure binary gradient system with a C18 guard column. Additives like acetic acid can contain a significant amount of iron. E.g. 100 ppb (parts per billion) may sound like a low level. However, 100 ppb = 100 ng/l or 100 pg/µl. Most current MS systems have specifications at much lower concentrations than this. E.g.. Reserpine 1pg/µL for many signal:noise specifications. Presence of metal ions in acetic acid can form adducts which produce intense peaks in ESI+ spectra. The use of additives can be a balance between the increase in sensitivity of the analyte compounds against the increase in the background ion intensities. b) Sample and solvent containers The following items can be sources of background ions i. Vials, caps, well plates 1. Waters vials are quality controlled. Brand X may not be as clean 2. Vial caps with septa may contain plastics or adhesives 3. Well plate glue-on foil covers may leach adhesives ii Glassware 1. Washing in a common dishwashing facility can contaminate glassware with detergent residues (PEG-like compounds) and surfactants. 2. Rinse only with mobile phase quality solvents that will be used _1 4 of 9
5 iii. Plastic containers or tubing Storage of solvents or water in plastic is not recommended as compounds may leach out of the container into the contents (e.g. dioctylphthalate contamination). c) Sample and sample matrix Sample matrix may contain salts and other unwanted materials. The solubility of the matrix must be considered when preparing needle wash solutions. i. Inorganic salts These are not soluble in high organic solvents. Buffers containing sodium (Na + ), potassium (K + ), phosphate (PO 4 3- ) should be avoided because they are not volatile. Substitution of ammonium (NH 4 + ),acetate or formate make the buffers volatile and MS compatible. d) Column ii Proteins Proteins (e.g. from tissues, blood or serum samples) will precipitate in high (>40%) organic solvents. The precipitated proteins can clog injectors and tubing. They can also adsorb the analyte or contaminates. iii. Sample Prep Sample preparation chemicals (e.g. detergents, salts) can produce large unwanted ions. Sample cleanup needs to be LC/MS friendly. iv. Solubility Analyte solubility can be a problem. If the sample is dissolved in high organic and then injected into initial mobile phase that is low in organic, some analyte could precipitate out of solution and contaminate the injector and/or the column. These species may then re-dissolve when a higher organic content gradient is subsequently introduced. v. Injector contamination Injection of very high concentrations of sample may contaminate the injector leading to sample carryover into the next injection. This can commonly occur when looking for impurities in the sample at 0.1% level where the main sample component may be very concentrated. HPLC columns can behave like a filter. Particles, precipitated proteins, etc. can stay at the head of the column and slowly bleed off, increasing the background ions. This is known as trace enrichment. i. Column types C18 analytical or trapping columns will trap hydrophobic compounds from water and will trace enrich them. Other column packings have different polarities that can trap different classes, e.g.. polar endcapped columns will retain more polar solutes. ii. Contaminant Chromatography Compounds trapped on the head of a HPLC column may elute as distinct LC peaks or as a smear across the chromatogram. iii. Trace Enrichment The trace enriching effect amplifies the amount of contamination present in the solvents or the HPLC system _1 5 of 9
6 d) Tubing iv. Equilibration pros and cons Equilibrating a C18 HPLC column for long periods of time at high aqueous will trap more contaminants. Methods requiring high aqueous conditions should be periodically cleaned with an organic mobile phase e.g. 70:30 acetonitrile:water. Ideally, a short equilibration time between samples is best, ensuring that the eluent is diverted to waste so any contaminants from the column do not flush into the MS. i. PEEK PEEK is a plastic polymer. Very hydrophobic compounds (e.g. steroids) can stick to it and contribute to contamination when they elute. Organic solvents can remove compounds (e.g. plasticizers) from the tubing, which subsequently show on the mass spectrum. It is sometimes useful to flush new PEEK tubing through with organic and aqueous solvents prior to connection to an MS. ii. Silica e) HPLC / UPLC System Silica capillary tubing has an active ion surface. Some compounds (e.g. some proteins and peptides) will stick to silica. Substances that stick to glass will probably stick to silica. When they elute they will contribute to contamination. i. Internal components, i.e. Tubing, Check Valves, Seals HPLC systems have multiple assemblies and other items that can accumulate contamination in small dead volumes. A thorough flush of the HPLC system with clean solvents can remove contaminants from the system. Sample needles, needle seals, syringes, rheodyne components etc can all contribute to background ions. Frit filters, sample filters, etc, should be replaced periodically. ii. External Tubing The tubing that connect the outlet of the HPLC system to the MS is easily replaced and can be easily troubleshooted as a potential source of background ions. iii. Solvent bottles, filters etc Solvent bottles should be washed thoroughly in a non-detergent cleaning agent, and thoroughly rinsed with those HPLC grade solvents which are to be subsequently used as mobile phases for sample analysis prior to use. Solvent bottles filters should be replaced periodically. iv. Pumps The pump and/or autosampler modules (e.g.. Acquity BSM, and SM) should be flushed with clean solvents, ensuring all solvent pathways have been selected at least once. Injector assemblies and syringes should be primed for at least cylces. v. Wash Solutions The following solutions have been used to clean LC systems (using HPLC or better grade solvents). Mixture 1: 25% Acetonitrile 25% Methanol 25% Water 25% Isopropanol 0.2 % Formic acid _1 6 of 9
7 Mixture 2: 50% Acetonitrile 49% Water 1% Ammonium Hydroxide f) MS System The use of strongly acidic wash solution are not generally recommended for cleaning LC systems are connected to MS systems, but if used the mixture should be thoroughly washed out of the system subsequently with water. Mixture 1 has been used as a strong universal wash solution, and can be used to do a precursor wash of an LC system during installation, if required. This mixture should be thoroughly flushed out of the system with another solution, e.g. 10:90 Acetonitrile:Water. Mixture 2 has been used to reduce PEG contamination, and should also be followed by a 10:90 Acetonitirle:Water solution after use. After any wash, it is recommended that mobile phase be washed through the system to equilibrate the LC and MS at initial conditions. Mass spectrometers can be used to analyse for many different types of sample. A portion of the samples admitted to the system can become stuck or deposit in various parts of the instrument. Typically 90% of all MS contamination can be removed by cleaning the source region as described in the instrument Operators Guide. Generally there is no need to go any further inside the instrument for routine maintenance cleaning. i. ESI / APCI probe / Corona Pin The probe is where the ions are created. Therefore, any contaminants present in this region are likely to ionise and be seen in the mass spectrum. Is it good practice to rebuild the ESI probe with new components e.g. Capillary, probe tip etc, to reduce the risk of contaminant build up. When troubleshooting contaminant location, it is useful to try a replacement probe. ii. Sample Cone The sample cone is the entry point of all ions into the MS. It is good practice to clean this periodically by sonicating in a 10% formic acid solution, followed by 50:50 Methanol:Water rinse. iii. Lockspray Components MS instruments with Lockspray have additional components that can accumulate contaminants. The Reference probe should be cleaned in the same way as the main analyte probe. The baffle can be cleaned as per the sample cone. iv. Sample lines/syringes The sample introduction flow path can be prone to build up of samples/matrices/impurities in solvents etc. It is recommended that the silica infusion line/peek fittings etc be changed frequently. The sample or lockspray syringe can be cleaned with solvents and/or mobile phase appropriate to the sample types that has been used. v. Ion guides and hexapoles Most Waters instruments use either ion guides or hexapoles to transport ions from the ion source to the analyser. Usually, at least one of these should be cleaned periodically refer to the specific instrument Operator s Guide. vi. Other MS assemblies MS systems contain other assemblies that may require cleaning from time to time. Most of these are only accessible by a trained engineer 34301_1 7 of 9
8 e.g.. Pre/post-filters and collision cells on quadrupole MS instruments, transfer lens assemblies on TOF MS instruments. Details of cleaning procedures can be found in instrument Techincal Support Note documents. NOTE: It is generally NOT recommended that quadrupole assemblies be cleaned on a customer site under normal circumstances. 3. Contamination Location Strategy The following table is a strategy for locating the source of background ions. Step Test 1 Can the background ions be tuned away. E.g, are they affected by sample cone voltage, ESI capillary voltage etc 2 Using a syringe pump fitted, directly infuse a sample of the mobile phase solutions (extracted from those solutions currently in use by the HPLC) 3 Put clean mobile phase mixture through each pump of the HPLC, UPLC or CapLC to the MS with no column at a low flow rate. Background Level Changes Constant High Low Higher Lower Next Action Contamination is external to MS. E.g. HPLC system Contamination may be on internal MS component. Go to cleaning procedures. a. Solvent, water, and or acid contaminated. Try different source of solvents and acid. b. Infusion kit, bottle or MS dirty. Clean or replace. Contamination is not in solvents or acid. Go to Step 3. HPLC system is contributing contamination. Go to Step 4. Not coming from the LC system. Go to Step 5. 4 If possible, disconnect the pump from the autosampler. Pump solvent mixture directly into MS using Inlet pump without autosampler. 5 Pump mobile phase mixture through the parts of the system, adding them one at a time tubing, filter(s), column(s). High Low High Contamination is in the pump. Go to cleaning procedures. Contamination is in the autosampler. Go to cleaning procedures. The lasted added component contains the contamination Go to cleaning procedures _1 8 of 9
9 iv. Other information It is often not possible to identify the last sample or conditions that introduced contamination to an LC/MS system. However, the general lab environment may provide an indication of possible sources of background ions. For example, questions to bear in mind could be: 1. What type of lab is this? Open access: Many different sample types, usually the same mobile phase conditions. Most open access labs keep a sample record with details of previous sample types, names, concentrations, matrices etc. R&D: Generally have a few target compounds under routine analysis. Has a new analysis study been started recently? Did the research project change recently? Purification / Trace analysis: Generally have small numbers of samples, but in large quantities/concentrations. May have to inject a concentrated sample to see impurities at <1% level. 2. What samples have been analysed? Is there a sample log? Have there been any new users of the LC/MS system recently? 3. Are there any other LC or MS systems in the room? If so, what samples are they running? Under what conditions? Could a more concentrated sample have been run on this instrument by mistake? 4. Have the solvent suppliers changed recently? Some manufactures solvents are not as clean as others. Has a new batch just been started? 5. Is the API gas supply pure? If possible, replace the supply with a bottled supply to rule out a contaminated N 2 supply. 6. How are solvent bottles cleaned? Is there a communal dishwasher? Are detergents or surfactants used? 34301_1 9 of 9
for Acclaim Mixed-Mode HILIC-1 Column
for Acclaim Mixed-Mode HILIC-1 Column Product Manual for ACCLAIM Mixed-Mode HILIC-1 Page 1 of 17 Product Manual for ACCLAIM Mixed-Mode HILIC-1 Column 5µm, 4.6 x 250mm, P/N 066844 5µm, 4.6 x 150mm, P/N
More informationAgilent G3212 GC-APCI Source
Agilent G3212 GC-APCI Source Quick Start Guide Where to find information 2 Getting Started 3 Step 1. Start the Data Acquisition program for the GC and the Q-TOF 3 Step 2. Prepare the GC and Q-TOF for data
More informationUPLC Intact MASS Analysis Application Kit
(Part Number: 176001519) CONTENTS I. INTACT MASS ANALYSIS APPLICATION KIT COMPONENTS II. INSTALLING THE PRE-COLUMN TUBING INTO MASSPREP MICRO DESALTING COLUMN III. CONNECTING THE COLUMN TO LCT PREMIER
More informationDetermination of trace anions in concentrated hydrofluoric acid
APPLICATION NOTE 78 Determination of trace anions in concentrated hydrofluoric acid Authors Archava Siriraks Thermo Fisher Scientific, Sunnyvale, CA Keywords HF, ICS-5000 +, IonPac AS10, IonPac AC10, ion
More informationLive Webinar : How to be more Successful with your ACQUITY QDa Detector?
Live Webinar : How to be more Successful with your ACQUITY QDa Detector? Q&A Transcript ---------------- Q - How do you generate multiple charges reproductively? A - If you use the same settings on the
More informationDetermination of urea in ultrapure water by IC-MS/MS
APPLICATION NOTE 72482 Determination of urea in ultrapure water by IC-MS/MS Authors Soon Fatt Lee, 1 Fiona Teh Hui Boon, 1 Chris Cheah Hun Teong, 1 and Jeff Rohrer 2 ¹Thermo Fisher Scientific, Singapore
More informationACQUITY UPLC HSS Columns
CONTENTS I. INTRODUCTION II. II. GETTING STARTED a. Column Connectors b. Column Installation c. Column Equilibration d. ecord Installation e. Initial Column Efficiency Determination f. VanGuard Pre-columns
More informationFAQ's. 1 - Which column would be the most appropriate for my application?
1 - Which column would be the most appropriate for my application? Due to the complexity of the chiral recognition mechanism, it is not possible yet to establish rules for the selection of the best chiral
More informationShodex TM ODP2 HP series columns
HPLC Columns Shodex TM ODP2 HP series columns Better retention of highly polar substances Technical notebook No. 6 Contents 1. Introduction 1-1. Specifications 1-2. Eluent Compatibility of ODP2 HP Series
More informationQTOF Training Manual
1236 Hach Hall 515-294-5544 www.cif.iastate.edu QTOF Training Manual (11/1/211 K.H.) Table of Contents Important Notes p.3 Overview of QTOF Hardware p.5 Overview of LC System p.5 Electrospray Ionization
More informationRoutine MS Detection for USP Chromatographic Methods
Daniel S. Root, Thomas E. Wheat, and Patricia McConville Waters Corporation, Milford, MA, USA APPLICATION BENEFITS This approach enables mass spectral analysis of peaks directly from unmodified USP HPLC
More informationBioanalytical Chem: 4590: LC-MSMS of analgesics LC-MS Experiment Liquid Chromatography Mass Spectrometry (LC/MS)
Liquid Chromatography Mass Spectrometry (LC/MS) Prelab Questions: Questions to be answered before doing the experiment. The answers are due at the beginning of each experiment without exception (the questions
More informationC18 Column. Care & Use Sheet
C18 Column Care & Use Sheet HALO Description HALO C18 is a high-speed, high-performance liquid chromatography column based on a new Fused-CoreTM particle design. The Fused-Core particle provides a thin
More informationM M e M M H M M H. Ion Sources
Ion Sources Overview of Various Ion Sources After introducing samples into a mass spectrometer, the next important step is the conversion of neutral molecules or compounds to gas phase ions. The ions could
More informationElectrospray Ion Trap Mass Spectrometry. Introduction
Electrospray Ion Source Electrospray Ion Trap Mass Spectrometry Introduction The key to using MS for solutions is the ability to transfer your analytes into the vacuum of the mass spectrometer as ionic
More informationThe Use of the ACQUITY QDa Detector for a Selective, Sensitive, and Robust Quantitative Method for a Potential Genotoxic Impurity
The Use of the ACQUITY QDa Detector for a Selective, Sensitive, and Robust Quantitative Method for a Potential Genotoxic Impurity Janet Hammond Waters Corporation, Wilmslow, UK APPLICATION BENEFITS High
More informationAnalysis of Metals, Halides, and Inorganic Ions Using Hydrophilic Interaction Chromatography
Application Note Inorganic Ions, Water Testing, Minerals, Metals, Basic Chemicals Analysis of Metals, Halides, and Inorganic Ions Using Hydrophilic Interaction Chromatography Authors Anne Mack, Adam Bivens
More informationikey Separation Device
ikey Separation Device CONTENTS I. INTRODUCTION II. III. IV. ikey SEPARATION DEVICE FEATURES a. Analytical ikey and ikey HT b. PCA ikey c. Accessory ikeys d. ikey Component Description CONNECTING AND REMOVING
More informationChemistry Instrumental Analysis Lecture 37. Chem 4631
Chemistry 4631 Instrumental Analysis Lecture 37 Most analytes separated by HPLC are thermally stable and non-volatile (liquids) (unlike in GC) so not ionized easily by EI or CI techniques. MS must be at
More informationDionex IonPac AS28-Fast-4µm column
CHROMATOGRAPHY Thermo Scientific Dionex IonPac AS-Fast-4µm Columns Product Specifications The Thermo Scientific Dionex IonPac AS-Fast-4µm column is a high-capacity, hydroxide-selective anionexchange column
More informationBasic principles of HPLC
Introduction to the theory of HPLC HPLC (High Performance Liquid Chromatography) depends on interaction of sample analytes with the stationary phase (packing) and the mobile phase to effect a separation.
More informationVALIDATION OF A UPLC METHOD FOR A BENZOCAINE, BUTAMBEN, AND TETRACAINE HYDROCHLORIDE TOPICAL SOLUTION
VALIDATION OF A UPLC METHOD FOR A BENZOCAINE, BUTAMBEN, AND TETRACAINE HYDROCHLORIDE TOPICAL SOLUTION Andrew J. Aubin and Tanya L. Jenkins Waters Corporation, Milford, MA, USA INTRODUCTION Benzocaine (4-Aminobenzoic
More informationCRL MASS SPECTROMETRY FACILITY USER MANUAL LCT CLASSIC A & B
Mass Spectrometry Instrument Training Guide Page 1 of 18 24/10/2012 CRL MASS SPECTROMETRY FACILITY USER MANUAL LCT CLASSIC A & B 1st Floor Mass Spec Lab: 00.097 This is a guide to using the LCT classic
More informationUnexpected Peaks in Chromatograms - Are They Related Compounds, System Peaks or Contaminations? From the Diary of an HPLC Detective
Unexpected Peaks in Chromatograms - Are They Related Compounds, System Peaks or Contaminations? From the Diary of an HPLC Detective SHULAMIT LEVIN HPLC in Pharmaceutics Σ Stability Indicating Methods Extra
More informationACQUITY UPLC Peptide BEH C 18, 130Å and 300Å Columns
CONTENTS I. INTRODUCTION II. III. GETTING STARTED a. Column Connectors b. Column Installation c. Column Equilibration d. ecord Installation e. Initial Column Efficiency Determination COLUMN USE a. Sample
More informationHPLC solvents and mobile phase additives
HPLC solvents and mobile phase additives The following is intended to be a guide for the choice of solvent and mobile phase additives. Of course the choice of solvents for LC will be dictated primarily
More informationCAPCELL PAK C18 IF2 Type http://hplc.shiseido.co.jp/e/column/html/if2_index.htm Page 1 of 2 List of Sales Representatives Contact Shiseido Technical Materials Catalog List HPLC Columns HPLC Instruments
More informationLC Technical Information
LC Technical Information Method Transfer to Accucore.6 μm Columns Containing solid core particles, which are engineered to a diameter of.6μm and a very narrow particle size distribution; Accucore HPLC
More informationUtilizing ELSD and MS as Secondary Detectors for Prep HPLC and Flash Chromatography. Tips and Techniques to Optimize ELSD and MS based Purification
Utilizing ELSD and MS as Secondary Detectors for Prep HPLC and Flash Chromatography Tips and Techniques to Optimize ELSD and MS based Purification Utilizing ELSD and MS as Secondary Detectors for Prep
More informationBEST PRACTICES IN THE ANALYSIS OF RAPIFLUOR-MS LABELED GLYCANS USING THE ACQUITY QDa DETECTOR (PERFORMANCE MODEL)
BEST PRACTICES IN THE ANALYSIS OF RAPIFLUOR-MS LABELED GLYCANS USING THE ACQUITY QDa DETECTOR (PERFORMANCE MODEL) The following document provides basic understanding and guidance in the configuration of
More informationThe end of. mass-speculation. MS Certified Vials Pre-cleaned and certified vials for mass spectrometry
The end of mass-speculation Pre-cleaned and certified vials for mass spectrometry Bonded, ultra-pure closures LC/MS and GC/MS Manufacturing the Ultimate Vial for Mass Spectrometry More than a quarter century
More informationAnalytical determination of testosterone in human serum using an Agilent Ultivo Triple Quadrupole LC/MS
Application Note Clinical Research Analytical determination of testosterone in human serum using an Agilent Ultivo Triple Quadrupole LC/MS Authors Yanan Yang 1, Victor Mandragon 2, and Peter Stone 1 1
More informationTraining Courses. Chromatography training from the Crawford Scientific experts
Training Courses Chromatography training from the Crawford Scientific experts HPLC Fundamentals This one-day course introduces the fundamentally important concepts associated with HPLC analysis including
More information[ CARE AND USE MANUAL ]
CONTENTS I. INTRODUCTION II. III. IV. GETTING STARTED a. Column Installation b. Column Equilibration c. Initial Column Efficiency Determination COLUMN USE a. Guard Columns b. Sample Preparation c. ph Range
More informationThe Agilent InfinityLab 2D-LC Solution with Active Solvent Modulation
Technical Overview The Agilent InfinityLab D-LC Solution with Active Solvent Modulation Achieving Improved Resolution and Sensitivity for Challenging Combinations of Separation Conditions Author Sonja
More informationProPac WCX-10 Columns
ProPac WCX-10 Columns Guidance for column use Tips to maximize column lifetime ProPac WCX-10 Column Tips and Tricks This guide provides essential information and invaluable guidelines for mobile phases,
More informationOpen Column Chromatography, GC, TLC, and HPLC
Open Column Chromatography, GC, TLC, and HPLC Murphy, B. (2017). Introduction to Chromatography: Lecture 1. Lecture presented at PHAR 423 Lecture in UIC College of Pharmacy, Chicago. USES OF CHROMATOGRAPHY
More informationChemistry Instrumental Analysis Lecture 31. Chem 4631
Chemistry 4631 Instrumental Analysis Lecture 31 High Performance Liquid Chromatography (HPLC) High Performance Liquid Chromatography (HPLC) High Performance Liquid Chromatography (HPLC) Solvent Delivery
More informationSolid Phase Extraction Method Development Tips and Tricks
Solid Phase Extraction Method Development Tips and Tricks Carol Haney Ball, Ph.D. Application Scientist Agilent Technologies, Inc. February 3, 2009 Sources of Error Generated and Time Spent During a Typical
More informationHigh Performance Liquid Chromatography
High Performance Liquid Chromatography What is HPLC? It is a separation technique that involves: Injection of small volume of liquid sample Into a tube packed with a tiny particles (stationary phase).
More information[ Care and Use Manual ]
XSelect High Strength Silica (HSS) hplc Columns Contents I. INTRODUCTION II. CONECTING THE COLUMN TO THE HPLC SYSTEM a. Column Connection b. Column Connectors and System Tubing Considerations c. Band Spreading
More informationBarry E. Boyes, Ph.D. Consumables and Accessories Business Unit May 10, 2000
Barry E. Boyes, Ph.D. Consumables and Accessories Business Unit May 0, 000 HPLC Column Troubleshooting What Every HPLC User Should Know :00 a.m. EST Telephone Number: 86-650-06 Chair Person: Tim Spaeder
More informationMaximizing Triple Quadrupole Mass Spectrometry Productivity with the Agilent StreamSelect LC/MS System
Maximizing Triple Quadrupole Mass Spectrometry Productivity with the Agilent StreamSelect LC/MS System Application Note Authors Kevin McCann, Sameer Nene, Doug McIntyre, Edmond Neo, Dennis Nagtalon, and
More informationMacrolides in Honey Using Agilent Bond Elut Plexa SPE, Poroshell 120, and LC/MS/MS
Macrolides in Honey Using Agilent Bond Elut Plexa SPE, Poroshell 120, and LC/MS/MS Application Note Food Testing and Agriculture Author Chen-Hao (Andy) Zhai and Rong-jie Fu Agilent Technologies (Shanghai)
More informationHigh Performance Liquid Chromatography
STANDARDBASE techniques: High Performance Liquid Chromatography Drenthe College, The Netherlands 1. Introduction HPLC. High Performance Liquid Chromatography High Performance Liquid Chromatography (HPLC)
More informationChapter content. Reference
Chapter 7 HPLC Instrumental Analysis Rezaul Karim Environmental Science and Technology Jessore University of Science and Technology Chapter content Liquid Chromatography (LC); Scope; Principles Instrumentation;
More informationTANDEM MASS SPECTROSCOPY
TANDEM MASS SPECTROSCOPY 1 MASS SPECTROMETER TYPES OF MASS SPECTROMETER PRINCIPLE TANDEM MASS SPECTROMETER INSTRUMENTATION QUADRAPOLE MASS ANALYZER TRIPLE QUADRAPOLE MASS ANALYZER TIME OF FLIGHT MASS ANALYSER
More informationLC-MS Based Metabolomics
LC-MS Based Metabolomics Analysing the METABOLOME 1. Metabolite Extraction 2. Metabolite detection (with or without separation) 3. Data analysis Metabolite Detection GC-MS: Naturally volatile or made volatile
More informationHPLC Columns. HILICpak VT-50 2D MANUAL. Shodex HPLC Columns Europe, Middle East, Africa, Russia
HPLC Columns MANUAL HILICpak VT-50 2D Shodex HPLC Columns Europe, Middle East, Africa, Russia For technical support please use contact details shown below: SHOWA DENKO EUROPE GmbH Shodex Business Konrad-Zuse-Platz
More informationLIQUID CHROMATOGRAPHY-MASS SPECTROMETRY (LC/MS) Presented by: Dr. T. Nageswara Rao M.Pharm PhD KTPC
LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY (LC/MS) Presented by: Dr. T. Nageswara Rao M.Pharm PhD KTPC INTRODUCTION Principle: LC/MS is a technique that combines physical separation capabilities of liquid
More informationTips and tricks to increase HPLC column lifetime. Dr. Frank Michel
Tips and tricks to increase HPLC column lifetime Dr. Frank Michel Overview How to influence HPLC column life time? HPLC method Helpful accessories Best practice 2 HPLC Method Mobile Phase Mobile phase
More informationDetermination of Trace Cations in Power Plant Waters Containing Morpholine
Application Note 8 Determination of Trace Cations in Power Plant Waters Containing Morpholine INTRODUCTION Morpholine and ammonium are used as additives in power plant waters. Morpholine acts as a corrosion
More informationLC Column Troubleshooting. Do you have an equivalent column for my LC column?
LC Column Troubleshooting Do you have an equivalent column for my LC column? LC columns from different suppliers may have very different retention properties even if the bonding is the same. Although there
More informationTechnical Procedure for Concentration Determination of Methamphetamine in Liquids via HPLC
Technical Procedure for Concentration Determination of 1.0 Purpose This procedure specifies the required elements for the preparation and use of the Agilent 1100/1200 series High Performance Liquid Chromatograph
More informationTR ACE ORGANIC. lgcstandards.com/foodandenvironment
U S E O F S TA B L E I S OTO P E I NTE R N A L S TA N D A R D S F O R TR ACE ORGANIC A N A LY S I S lgcstandards.com/foodandenvironment dr.ehrenstorfer@lgcgroup.com This paper explains why stable isotope
More informationANALYTICAL METHOD DETERMINATION OF VOLATILE ALDEHYDES IN AMBIENT AIR Page 1 of 11 Air sampling and analysis
DETERMINATION OF VOLATILE ALDEHYDES IN AMBIENT AIR Page 1 of 11 Replaces: Dated: Author: Date: AM-No.: New New Nils Arne Jentoft 18.06.2014 0 CHANGES This procedure is new. 1 SCOPE This document describes
More information[ CARE AND USE MANUAL ] XSELECT HSS XP 2.5 µm COLUMNS I. INTRODUCTION CONTENTS I. INTRODUCTION II. GETTING STARTED III. COLUMN USE
XSELECT HSS XP 2.5 µm COLUMNS CONTENTS I. INTRODUCTION II. GETTING STARTED a. Column Connection b. Column Installation c. Minimizing Band Spread Volume d. Measuring Band Spread Volume e. Measuring System
More informationIntroduction of Hitachi Chromaster 5610 MS Detector for High Performance Liquid Chromatograph
SCIETIFIC ISTRUMET EWS 2016 Vol. 7 SEPTEMBER Technical magazine of Electron Microscope and Analytical Instruments. Technical Explanation Introduction of Hitachi Chromaster 5610 MS Detector for High Performance
More informationAcclaim Mixed-Mode WAX-1 Columns
User Manual Acclaim Mixed-Mode WAX- Columns 06565 Revision 03 October 05 Product Manual for the Acclaim Mixed-Mode WAX- Column Page of 3 Product Manual for Acclaim Mixed-Mode WAX- Columns 5µm, 0 x 50 mm,
More informationMass Spectrometry in MCAL
Mass Spectrometry in MCAL Two systems: GC-MS, LC-MS GC seperates small, volatile, non-polar material MS is detection devise (Agilent 320-MS TQ Mass Spectrometer) Full scan monitoring SIM single ion monitoring
More information[ Care and Use Manual ]
high Strength Silica hplc Columns Contents I. INTRODUCTION II. CONECTING THE COLUMN TO THE HPLC SYSTEM III. Waters Small Particle Size (3.5 m) Columns Fast Chromatography IV. Column Equilibration V. Column
More informationProudly serving laboratories worldwide since 1979 CALL for Refurbished & Certified Lab Equipment
www.ietltd.com Proudly serving laboratories worldwide since 1979 CALL +1.847.913.0777 for Refurbished & Certified Lab Equipment Applied Biosystems QStar Pulsar i Features of the API QSTAR Pulsar i The
More informationChromatography. Gas Chromatography
Chromatography Chromatography is essentially the separation of a mixture into its component parts for qualitative and quantitative analysis. The basis of separation is the partitioning of the analyte mixture
More informationIonPac Trace Cation Concentrator
for the IonPac Trace Cation Concentrator (TCC-LP1, TCC-ULP1 and TCC-XLP1) Page 1 of 17 PRODUCT MANUAL FOR TRACE CATION CONCENTRATOR (TCC) TCC-LP1 Column Low Pressure, 4 x 35 mm (P/N 046027) TCC -ULP1 Column
More informationCalibrating Thermo Exactive with the Direct Analysis in Real Time (DART) Ambient Ionization Source (Protocol Adapted from US FDA FCC)
1.0 Equipment: Calibrating Thermo Exactive with the Direct Analysis in Real Time (DART) Ambient Ionization Source (Protocol Adapted from US FDA FCC) Thermo Exactive Orbitrap Mass Spectrometer Direct Analysis
More informationfor Acclaim Trinity TM P1
for Acclaim Trinity TM P Product Manual for Acclaim TRINITY P Columns Page of 4 Product Manual for Acclaim Trinity TM P Columns 07556 Acclaim Trinity P, 3µm, 4.6 x 00mm 07556 Acclaim Trinity P, 3µm, 4.6
More informationLC/MS/MS qua ntitation of β-estradiol 17-acetate using an Agilent 6460 Triple Quadrupole LC/MS working in ESI negative ion mode
LC/MS/MS qua ntitation of β-estradiol 17-acetate using an Agilent 6460 Triple Quadrupole LC/MS working in ESI negative ion mode Application Note Authors Siji Joseph Agilent Technologies India Pvt. Ltd.
More informationAcclaim Mixed-Mode WCX-1
Acclaim Mixed-Mode WCX-1 Product Manual for the Acclaim Mixed-Mode WCX-1 Column Page 1 of 28 PRODUCT MANUAL for the Acclaim Mixed-Mode WCX-1 Columns 4.6 x 150 mm, P/N (068353) 4.6 x 250 mm, P/N (068352)
More informationBritish American Tobacco Group Research & Development. Method - Determination of ammonia in mainstream smoke
British American Tobacco Group Research & Development Method - Determination of ammonia in mainstream smoke 1 SCOPE OF APPLICATION The method is applicable to quantitative determination of the yields of
More informationAPI Optimization, Source Design, and Other Considerations of LC/MS
API Optimization, Source Design, and Other Considerations of LC/MS Instrument Design Considerations: The Atmosphere-Vacuum Interface and Pumping System The hows and whys of the vacuum? We ve got to get
More informationVolumetric Analysis. Quantitative analysis answers the second question
Volumetric Analysis Volumetric analysis is a form of quantitative analysis involving the measuring of volumes of reacting solutions, it involves the use of titrations. When buying food we often have two
More informationAgilent LC & LC-MS Cannabis Testing
Agilent LC & LC-MS Cannabis Testing Potency Analysis for Cannabinoids Mike Adams 1, A. Roth 1, Joan Stevens 2, Karen Kaikaris 1, & Sue D Antonio 2 1 CWC LABS, 2 Agilent Technologies, UV detection with
More informationIt s hot! ZIC -chilic
It s hot! ZIC -chilic Complementary selectivity for HPLC and LC-MS separation of polar hydrophilic compounds EMD Millipore Corp. is a subsidiary of Merck KGaA, Darmstadt, Germany ZIC -chilic Your benefits
More informationLC III: HPLC. Originally referred to as High-Pressure Liquid Chromatography. Now more commonly called High Performance Liquid Chromatography
LC III: HPLC What is HPLC? Originally referred to as High-Pressure Liquid Chromatography Now more commonly called High Performance Liquid Chromatography In general: The instrument controlled version of
More informationHigh Pressure/Performance Liquid Chromatography (HPLC)
High Pressure/Performance Liquid Chromatography (HPLC) High Performance Liquid Chromatography (HPLC) is a form of column chromatography that pumps a sample mixture or analyte in a solvent (known as the
More informationDetermination of Volatile Substances Proof of Food Adulteration
ANALYSIS OF FOOD AND NATURAL PRODUCTS LABORATORY EXERCISE Determination of Volatile Substances Proof of Food Adulteration (method: gas chromatography with mass spectrometric detection) Exercise guarantor:
More informationOVERVIEW INTRODUCTION. Michael O Leary, Jennifer Gough, Tanya Tollifson Waters Corporation, Milford, MA USA
Use of High Speed/High Resolution Size-Based Chromatographic Separation of Surfactants and Oligomeric Materials with Single Quadrupole Mass Spectrometry Michael O Leary, Jennifer Gough, Tanya Tollifson
More informationHPLC analysis of VFAs, Furfural and HMF
HPLC analysis of VFAs, Furfural and HMF Introduction The following chromatographic analysis is developed in order to analyse volatile fatty acids and carbohydrate degradation products; furfural, hydroxymethylfurfural
More informationSupporting information Online HPLC-ESI-HRMS Method for the Analysis and Comparison of Different Dissolved Organic Matter Samples
1 2 3 4 5 6 Supporting information Online HPLC-ESI-HRMS Method for the Analysis and Comparison of Different Dissolved Organic Matter Samples Claudia Patriarca a, *, Jonas Bergquist a, Per J. R. Sjöberg
More informationAgilent 1290 Infinity Quaternary LC Stepwise Transfer to Methods with MS-Compatible Mobile Phases
Agilent 129 Infinity Quaternary LC Stepwise Transfer to Methods with MS-Compatible Mobile Phases Technical Overview Author A.G.Huesgen Agilent Technologies, Inc. Waldbronn, Germany Abstract The Agilent
More informationHigh Performance Liquid Chromatography
Updated: 3 November 2014 Print version High Performance Liquid Chromatography David Reckhow CEE 772 #18 1 HPLC System David Reckhow CEE 772 #18 2 Instrument Basics PUMP INJECTION POINT DETECTOR COLUMN
More informationHigh Performance Liquid Chromatography
Updated: 3 November 2014 Print version High Performance Liquid Chromatography David Reckhow CEE 772 #18 1 HPLC System David Reckhow CEE 772 #18 2 1 Instrument Basics PUMP INJECTION POINT DETECTOR COLUMN
More informationRapid Screening and Confirmation of Melamine Residues in Milk and Its Products by Liquid Chromatography Tandem Mass Spectrometry
Rapid Screening and Confirmation of Melamine Residues in Milk and Its Products by Liquid Chromatography Tandem Mass Spectrometry Application Note Food Authors Jianqiu Mi, Zhengxiang Zhang, Zhixu Zhang,
More informationConc n of A OAs present (um) Conc n of B OAs present (um)
Materials and Instrumentation: Acquity UPLC BEH C18 2.1 x 100 mm, 1.7 µm column, Waters Corporation, Cat. No. 186002352 O-Benzylhydroxylamine, Sigma-Aldrich Cat. No. B22984 N-(3-Dimethylaminopropyl)-N
More informationDetermination of Polymer Modifier in Asphalt
Standard Method of Test for Determination of Polymer Modifier in Asphalt AASHTO Designation: T xxx-xx (2005) 1. SCOPE 1.1. This method of test is used to determine the polymer content of an asphalt sample.
More informationHPLC-MS of the Initial Perfluorinated Surfactants and Shorter Chains:
Details of the Analytical Procedures and Reactor Configurations. HPLC-MS of the Initial Perfluorinated Surfactants and Shorter Chains: Analysis for initial PF surfactant and possible shorter-chain products
More informationSimplified Approaches to Impurity Identification using Accurate Mass UPLC/MS
Simplified Approaches to Impurity Identification using Accurate Mass UPLC/MS Marian Twohig, Michael D. Jones, Dominic Moore, Peter Lee, and Robert Plumb Waters Corporation, Milford, MA, USA APPLICATION
More informationOMCL Network of the Council of Europe QUALITY MANAGEMENT DOCUMENT
OMCL Network of the Council of Europe QUALITY MANAGEMENT DOCUMENT PA/PH/OMCL (11) 04 QUALIFICATION OF EQUIPMENT ANNEX 1: QUALIFICATION OF HPLC EQUIPMENT Full document title and reference Document type
More informationMODERN HPLC FOR PRACTICING SCIENTISTS
MODERN HPLC FOR PRACTICING SCIENTISTS Michael W. Dong Synomics Pharmaceutical Services, LLC Wareham, Massachusetts WILEY- INTERSCIENCE A JOHN WILEY & SONS, INC., PUBLICATION Preface xv 1 Introduction 1
More informationOptimizing Mobile Phase Solvent Purity for LCMS
Optimizing Mobile Phase Solvent Purity for LCMS Thermo Fisher Scientific 6/3/09 Dannie Mak 1, Bryan Krastins 2, Eric Genin 3, Vincent Jespers 4, and Steve Roemer 1 1 Fair Lawn, NJ, USA 2 Cambridge, MA,
More informationWebinar: How to be More Successful with your ACQUITY QDa Detector Eric van Beelen
Webinar: How to be More Successful with your ACQUITY QDa Detector Eric van Beelen 2015 Waters Corporation 1 We are here to address any Questions you may have That s the benefit of participating to the
More informationChoosing the metabolomics platform
GBS 748 Choosing the metabolomics platform Stephen Barnes, PhD 4 7117; sbarnes@uab.edu So, I have my samples what s next? You ve collected your samples and you may have extracted them Protein precipitation
More informationcolumns IonPac AS17-C Anion Exchange Column
columns IonPac AS-C Anion Exchange Column The IonPac AS-C is a hydroxide-selective anion exchange column designed for fast gradient separation of inorganic anions. The key application for the AS-C column
More informationQuantitative Analysis of EtG and EtS in Urine Using FASt ETG and LC-MS/MS
Quantitative Analysis of EtG and EtS in Urine Using FASt ETG and LC-MS/MS UCT Part Numbers: CSFASETG203 - CLEAN SCREEN FASt ETG, 200mg / 3mL tube SLETG100ID21-3UM - Selectra ETG HPLC column, 100 x 2.1
More informationLC800. Smart HPLC. Until now UHPLC From now Smart HPLC
LC800 Smart HPLC Until now UHPLC From now Smart HPLC Smart HPLC Leads to Ultimate Performance Patent Pending S LC800 is a completely new and unique concept, designed for maximum performance in high resolution
More informationDe Novo Metabolite Chemical Structure Determination. Paul R. West Ph.D. Stemina Biomarker Discovery, Inc.
De Novo Metabolite Chemical Structure Determination Paul R. West Ph.D. Stemina Biomarker Discovery, Inc. As a part of non targeted metabolomic analysis, when peaks in the mass spectra are thought to be
More informationDEVELOPMENT OF PFCs HIGH SENSITIVITY ANALYSIS METHOD APPLIED RETENTION GAP TECHNIQUE WITH UPLC/MS/MS Tatsuya Ezaki 1, Nobutake Sato 1, Jun Yonekubo 1,
DEVELOPMENT O PCs HIGH SENSITIVITY ANALYSIS METHOD APPLIED RETENTION GAP TECHNIQUE WITH UPLC/MS/MS Tatsuya Ezaki 1, Nobutake Sato 1, Jun Yonekubo 1, Takeshi Nakano 2 1 Nihon Waters K.K,.1-3-12 Kitashinagawa,
More informationSupporting Information
Supporting Information Synthesis of a new class of ribose functionalized dinucleotide cap analogues for biophysical studies on interaction of cap-binding proteins with the 5 end of mrna. Karolina Piecyk,
More informationPerfluorinated Alkyl Acids (PFAA) in Water by LC/MS/MS - PBM
Organics Revision Date: July 19, 2017 Perfluorinated Alkyl Acids (PFAA) in Water by LC/MS/MS - PBM Parameter Perfluorinated Alkyl Acids (Perfluorobutane Sulphonate (PFBS), Perflourooctane Sulphonate (PFOS),
More informationHigh-Resolution Sampling 2D-LC for Pharmaceutical Impurity Analysis
High-Resolution Sampling D-LC for Pharmaceutical Impurity Analysis Detection of Impurities Hidden Under the API Peak at Relevant Levels Application Note Small Molecule Pharmaceuticals and Generics Authors
More information