Environmental Laboratory Workflow

Transcription

1 Environmental Laboratory Workflow

2 [ Environmental Laboratory Workflow ] sampling lab receives samples sample pretreatment sam extra RE-SAMPLING

3 The analysis of environmental samples involves a series of interconnected steps, each acting to produce and track information related to the samples to be analyzed. Samples must first be obtained and preserved in the proper manner while being delivered to the testing facility. Proper receiving and processing of the samples is critical to maintaining the chain of custody required by governmental agencies. The analysis must include all of the proper steps in order to produce the highest quality results. Results must be verified and approved before issuing a final report. The effective management and execution of each of these interactions results in the efficient analysis of each individual sample. Waters Corporation is at the forefront of environmental sample analysis and is proud to partner with laboratory professionals to effectively manage their analytical processes. Providing cutting-edge analytical solutions, including instrumentation, sample preparation, certified reference standards, proficiency testing and informatics, Waters ensures the efficient production of compliant data for a wide variety of environmental testing needs. RE-TEST ple ction analysis results reviewed final approval/ report generation

4 Environmental Analysis Laboratory Laboratory Workflow Workflow The amount of material, storage conditions, and holding times vary from method to method, largely depending on the compounds of interest, as well as the sample matrix. Generally, it is recommended to use amber glass sample containers to minimize external contamination and use sample sizes large enough to accommodate the analysis of multiple replicates. For greater accuracy of the final results, it is recommended to minimize handling of the samples, as well as holding times. Selected examples taken from established regulatory methods. Pharmaceuticals in Water 1. Collect L of water (if residual chlorine is present, add 80 mg sodium thiosulfate).. Store samples in dark at less than 10 C until analyzed. 3. Analyze within 40 days. 4. Some compounds may degrade rapidly in aqueous samples, therefore, is it strongly encouraged to complete the analysis within 48 hours. Pharmaceuticals in Soil 1. Collect samples using wide-mouth jars.. Collect a minimum of 10 g of dry soil. 3. Maintain soil samples in the dark at less than 6 C from time of collection until receipt at the laboratory. 4. Some compounds may degrade rapidly in soil samples, therefore, is it strongly encouraged to complete the analysis within 48 hours. Aldehydes in Air 1. Assemble sampling system for either a single-port or multi-port sampler using DNPH-coated cartridges.. Check system for leaks and to ensure it is operating properly. 3. In general, use flow rates of 1- L/min. 4. Operator must measure/record sampling flow rate at the beginning and end of the sampling period. 5. Sampler is turned on and operated for desired period. 6. Immediately after sampling, remove cartridge, cap and store. 7. Refrigerate at 4 C until analysis. 8. Storage should not exceed weeks. XPoSure Aldehyde Sampler Cartridges Ozone Scrubber Cartridge DNPH-Silica Cartridges [ 4 ]

5 Environmen tal L abor ator y Workf l ow Commercial testing laboratories generally supply sampling material and appropriate shipping supplies (coolers, insulated boxes) along with the necessary documentation for submitting samples for analysis. In most cases, this will include the appropriate change-of-custody forms which are required for local, state, and federal regulations. In addition, samples which may present health hazards or require special handling need to be clearly marked. Upon arrival, the samples are logged into the laboratory s LIMS system or appropriate tracking software. T he appropriate analyses are noted and when required, sub-samples are taken. T he sample and sub-samples are then transported to the appropriate department (Microbiology, W ET Chemistry, Organics, Inorganics, Metals) for analysis. NOT E: For the purposes of regulatory testing, the laboratory must demonstrate t he ability to carry out eac h met hod wit h acceptable precision and recovery. ERA Proficiency Testing Products Informatics Software [ 5 ] Informatics/Software

6 Environmental Laboratory Workflow Many samples require pretreatment prior to extraction. This is done in order to ensure the accurate and successful quantitation of the compounds of interest. Depending on the compounds and sample matrix, pretreatment could involve ph adjustment, sonication, centrifugation, or simple filtration. Certified LC/MS Vials DNPH-Silica Cartridges Pharmaceuticals in Water 1. Samples with no visible particles: a) Divide sample into two aliquots. b) Adjust one aliquot to ph.0 ± 0.5. c) Adjust the second aliquot to ph 10.0 ± Samples with visible particles: a) Filter the sample with filtration apparatus. Collect the aqueous fraction and prepare as above. b) Retain the filtrate and analyze using method for soil/solid analysis below. Pharmaceuticals in Soil 1. Homogenize sample in its original container (shaking, stirring, or similar).. Collect two aliquots equal to 1.0 g of dry material or a maximum of 5.0 g of wet weight. 3. Designate one sample as the acid fraction and one as the base fraction. 4. Acid fraction: a) Add 15 ml of ph phosphate buffer. b) Vortex for 5 min. c) Check and adjust ph to.0 ± 0.5 with buffer, vortexing as necessary. 5. Base fraction: a) Add 15 ml of reagent water. b) Vortex for 5 min. c) Check and adjust ph to 10.0 ± 0.5 by adding NH 4 OH solution, vortexing as necessary. Aldehydes in Air 1. Backflush sample cartridge with 5 ml of acetonitrile.. Label sample and store in refrigerated conditions until sample is analyzed by HPLC/UPLC. [ 6 ]

7 Environmental Laboratory Workflow T he extraction of the compounds of interest from the sample matrix serves multiple purposes. It removes interfering compounds of interest to ensure a more accurate analysis. It also concentrates the compounds to improve the sensitivity of the analysis. Finally, it can transfer the compounds into a solvent solution which is compatible with the analytical technique to be used. Commonly, sample extraction is performed using solid-phase extraction (SPE) or liquid-liquid extraction (LLE). Oasis SPE Cartridges Certified LC/MS Vials Certified Sep-Pak Cartridges Extraction Manifold Pharmaceuticals in Water 1. Assemble SPE extraction apparatus and attach Oasis SPE HLB cartridges.. Condition with 0 ml methanol and 6 ml reagent water. 3. When extracting acid fraction, condition with 6 ml reagent water at ph.0 ± Load sample onto cartridge flow rate 5-10 ml/min. 5. Wash acid fraction with 10 ml reagent water. (Do not wash cartridge for base fraction). 6. Dry cartridges under vacuum for 5 min. 7. Elute Acid fraction with 1 ml methanol. 8. Elute Base fraction with 6 ml methanol followed by 9 ml % formic acid. 9. Concentrate both acid and base frictions and exchange both fractions to methanol for analysis. Pharmaceuticals in Soil 1. Acid fraction: a) Add 0 ml ACN, sonicate for 30 min. followed by centrifugation for 5 min at 3000 rpm. b) Decant extracts into clean flask. c) Add 15 ml phosphate buffer to ample. Adjust to ph.0 ± 0.5 with HCl. Vortex to re-suspend solids. d) Perform a second extraction by repeating steps a-c. e) For the third extraction add 15 ml of ACN to each tube. f) Concentrate acid extraction, followed by aqueous SPE procedure as stated in the water sample above.. Base fraction: a) Add 0 ml ACN, sonicate for 30 min followed by centrifugation for 5 min at 3000 rpm. b) Decant extracts into clean flask. c) Add 15 ml reagent water. Add NH 4 OH to sample dropwise to adjust ph to 10.0 ± 0.5. Vortex as needed. d) Perform a second extraction by repeating steps a-c. e) For the third extraction, add 15 ml of ACN to each tube. f) Concentrate base extraction, followed by aqueous SPE procedure as stated in the water sample above. Aldehydes in Air No SPE required [ 7 ]

8 Environmental Laboratory Workflow The method of analysis varies by compounds, matrix, and even by region. For samples that are subject to regulatory review, the analysis method must adhere to local regulations and, in most instances, little deviation is allowed. ACQUITY UPLC System with TQ Detector ERA Certified Reference Standards Alliance HPLC System Informatics/Software HPLC and UPLC Columns Pharmaceuticals in Water 1. Analysis is performed by LC/MS/MS.. Establish the same operating conditions appropriate to the fraction and compound to be analyzed. 3. Analysis is performed using positive electrospray ionization (ESI+) for the acid fraction, as well as the base fraction analytes. 4. Inject the volume of concentrated extract into the LC/MS/MS instrument. Pharmaceuticals in Soil 1. Analysis is performed by LC/MS/MS.. Establish the same operating conditions appropriate to the fraction and compound to be analyzed. 3. Analysis is performed using positive electrospray ionization (ESI+) for the acid fraction, as well as the base fraction analytes. 4. Inject the volume of concentrated extract into the LC/MS/MS instrument. Aldehydes in Air 1. HPLC system is assembled and calibrated as described.. Prior to each analysis, check detector baseline to ensure stable conditions. 3. Prepare mobile phase as indicated in method, place in solvent reservoir, and set pump flow. 4. Inject 100 μl aliquot of sample. [ 8 ]

9 Environmen tal L abor ator y Workf l ow Generated data is subject to acceptance criteria relating to precision and accuracy often mandated in the regulatory SOP or methodology. Blanks, as well as spiked samples, are run alongside the unknown samples to ensure that highest quality data. Should the results not meet the required guidelines, the sample can be retested, or if necessary or appropriate, a new sample may be requested. 1. Penicillin µg/l. Diphenhydramine µg/l 3. Erythromycin µg/l 4. Carbamazapine µg/l 5. Oxacillin µg/l 6. Miconazole µg/l 4 Informatics/Software % ERA Certified Reference Standards Pharmaceuticals in Water min Naproxen 0.30 µg/l Warfarin 0.15 µg/l Ibuprofen 1.5 µg/l Triclosan 3.0 µg/l % % Penicillin µg/l. Diphenhydramine µg/l 3. Erythromycin µg/l 4. Carbamazapine µg/l 5. Oxacillin µg/l 6. Miconazole µg/l Pharmaceuticals in Soil min Naproxen 0.30 µg/l Warfarin 0.15 µg/l Ibuprofen 1.5 µg/l Triclosan 3.0 µg/l min Aldehydes in Air % Albuterol µg/l Cimetidine µg/l min 8. Methacrolein 9. Butanal 10. Benzaldehyde 11. Pentanal 1. M-tolualdehyde 13. Hexanal Formaldehyde Acetaldehyde Acetone Acrolein Propanol Crotonaldehyde MEK AU ppm standard AU % ppb standard.00 0 AU.004 CH3CN blank min 0 [ 9 ] min

10 Environmental Laboratory Workflow If the results meet the specified criteria, they are approved and passed along for approval in the final report. TargetLynx Application Manager Often samples which are submitted for regulatory purposes undergo a series of tests before a final report can be generated. Once all of the indicated or required testing has been concluded, a final report is generated and provided to the person submitting the original sample. [ 10 ] Informatics/Software

11 Environmen tal L abor ator y Workf l ow Waters Environmental Applications Perchlorates Perflourinated Compounds (PFOS/ PFOA) Carbamates Explosives Phenylurea Compounds Endocrine Disruptors Acetamide Herbicide Degradates Bisphenol A Chloracetanilide Endothall Olyphosate Organochlorine Pesticides Diquat/ Paraquat Petroleum Hydrocarbons Poly Aromatic Hydrocarbons (PAHs) Nitrogen, Phosphorus Pesticides Carbonyl Compounds Chlorinated Pesticides Pharmaceuticals and Personal Care Products Organic Compounds Nitroaromatics/Nitramines Chlroacetanilide, Acetamide Herbicide Aldehydes/Ketones Haloacetic Acids, Dalapon [ 11 ]

12 Sales Offices Austria and European Export (Central South Eastern Europe, CIS and Middle East) Australia Belgium Brazil Canada x05 China CIS/Russia Czech Republic Denmark Finland France Germany Hong Kong The Netherlands Norway Poland Puerto Rico Singapore Spain Sweden Switzerland Taiwan United Kingdom All other countries: Waters Corporation U.S.A Hungary India and India Subcontinent Ireland Italy Japan Korea Mexico The quality management system of Waters manufacturing facilities in Taunton, Massachusetts and Wexford, Ireland complies with the International Standard ISO 9001:000 Quality Management and Quality Assurance Standards. Waters quality management system is periodically audited by the registering body to ensure compliance. 009 Waters Corporation. Waters, The Science of What s Possible, Oasis, Alliance, UPLC, ACQUITY UPLC, Sep-Pak, ERA, TargetLynx and XPoSure are trademarks of Water Corporation EN October 009 KK-FP