Field sample preparation

A preparation batch is a group of up to 20 field samples, prepared together for the same analysis using the same lots of reagents and associated with common QC samples. In addition to field samples, a preparation batch must, at a minimum, include a method (extraction or digestion) blank, an LCS, and an LCSD. Other laboratory QC checks may be part of the preparation batch, such as an MS/MSD pair or a laboratory duplicate. If laboratory QC checks in a preparation batch meet the laboratory acceptance criteria, the batch is considered be in a state of control and every sample in it is acceptable, provided that individual QC checks are also acceptable. If the method blank and the samples in a preparation batch show contamination that makes sample results inconclusive or if the LCS and LCSD recoveries are not acceptable, the whole batch may be prepared again. 

The STM uses this eflFect to obtain a measurement of the surface by raster scanning over the sample in a manner similar to AFM while measuring the tunneling current. The probe tip is typically a few tenths of a nanometer from the sample. Individual atoms and atomic-scale surface structure can be measured in a field size that is usually less than 1 pm x 1 pm, but field sizes of 10 pm x 10 pm can also be imaged. STM can provide better resolution than AFM. Conductive samples are required, but insulators can be analyzed if coated with a conductive layer. No other sample preparation is required. 

Whilst for the analysis of plant material for cannabinoids both GC and HPLC are commonly used, in analytical procedures the employment of GC-based methods prevails for human forensic samples. Nonetheless, the usage of HPLC becomes more and more of interest in this field especially in combination with MS [115-120]. Besides the usage of deuterated samples as internal standards Fisher et al. [121] describe the use of a dibrominated THC-COOH (see 7.5). The usage of Thermospray-MS and electrochemical detection provide good performance and can replace the still-used conventional UV detector. Another advantage in the employment of HPLC rather than GC could be the integration of SPE cartridges, which are needed for sample preparation in the HPLC-system. 

Repeatability is defined as precision under conditions where independent test results are obtained with the same method on identical test material in the same laboratory by the same operator using the same equipment within short intervals of time. The replicate analytical portion for testing can be prepared from a common field sample containing incurred residues. This approach is used extremely rarely. Normally, repeatability is estimated by the relative standard deviation ofrecoveries, which should be lower than 20% per commodity and fortification levels according to SANCO/825/00. In justified cases, higher variability can be accepted. 

Sample preparation by contract research organization. In Japan, GLP for field residue study work has not yet been established and sample preparation for residue studies by private companies is not authorized. Contract research organizations are limited to prefectural research institutes and MAFF-recognized local research institutes, mainly neutral organizations, such as the Japan Plant Protection Association (JPPA). 

A system of record keeping must be used which eliminates any risk of confusing the samples. As a rule, samples should be recorded immediately after their arrival and, especially in the case of nonfrozen field samples, prior to preparation for analysis. A record should also be kept of the condition of the samples upon arrival at the receiving laboratory and of any packaging or labeling defects. 

The chemical preservation of a sample is dependent on the chemistry of the ground-water (e.g., pH) and on the chemical characteristics of the pesticide being studied. Preservatives can be added to the sample containers in the field or prepared in advance at the laboratory. To determine the need for a chemical preservative in the field (i.e., pH analyses), test the groundwater collected during the purging process and not the sample collected for analysis. 

Audits of each phase of the study should include personnel training, preparation of collection forms, application calibration, each sample collection procedure, sample transport, each type of chemical analysis, data recording, data entry, data verification and data storage. Data collection in the field is often tedious if automated logging devices are not in place. To ensure data integrity, the paper and ink used for field studies should be waterproof. Each data collection form should contain appropriate locations for information detailing the time and location of sample collection, sample transport and sample analysis. Data collection forms should be stored in an orderly fashion in a secure location immediately upon return of field teams from the field at the end of each day. It is also important for data quality for studies to collect necessary field data seven days per week when required. In our experience, poor study quality is likely when field sample and data collection do not proceed on weekends. 

Travel fortification samples are a type of field fortification that is usually prepared in the fleld to allow the investigator to determine the stability of the active ingredient on matrices without weathering. Such matrices are fortified and placed immediately in frozen storage. Usually, one set of travel fortification samples for each matrix is prepared for each five sets of weathered fleld fortification samples. The samples are then stored and shipped using the same procedures as all other samples prepared in the fleld. 

J. Pawliszyn (ed.), Sampling and Sample Preparation for Field and Laboratory, Elsevier, Amsterdam (2003). 

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