HORIZONTAL Factsheet
Pharmaceuticals
version: 2/12/2016
SUBJECT
Determination of PHARMACEUTICALS
HORIZONTAL number
26
Matrices
Soil, sludge, waste…..
Existing standards used as basis
Work package
..........................................
CEN/TC 292, CEN/TC 308, CEN/TC 345, ISO/TC
190
5 Organic parameters
Project
STREP FP6 HORIZONTAL-ORG
Expert
Dr. Johanne Beausse
Organisation
Anjou Recherche
Country
France
Email
johanne.beausse@generale-des-eaux.net
Standardisation Committees
Status
Desk study First
Comments Phase I
Final version
Ruggedness Phase II
Second consultation
July 2004
December 2004
………
www.ecn.nl/horizontal
Completion due 30-09-05
Completion due 31-12-05
Validation
Transfer to BT/TF151
Foreseen 31-12-05
Summary of PHARMACEUTICALS procedure
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Regarding the differences in physical and chemical properties of the studied compounds,
three analytical methods are developed : antibiotics, others pharmaceuticals and steroids
hormones.
The development for steroids is finished. The sample preparation and the analytical
parameters were optimised. The steroid hormones were analysed using LC-MS/MS. The
sample preparation consists on one extraction step using soxtec and two purification steps on
SPE cartridges (C18 and Florisil). The performances of the method have been studied in term
of limits of quantification and repeatability. Steroids can be analysed from 0.5 ng/g or 1 ng/g
depending of the compounds.
Concerning the antibiotics and other pharmaceuticals, methods are still being developed. The
analytical parameters were optimised and currently the sample preparation is being
developed. Different extraction techniques and extraction solvents have been tested. Due to
the degradation of some compounds during the extraction, the soxtec technique is not retained
for the extraction. For the optimisation of the extraction, the next step will concern the
evaluation of ASE and sonication with the selected extraction solvent. One purification step
on SPE cartridge (SAX/HLB) was optimised.
Concerning the development of the method for the analysis of antibiotics and other
pharmaceuticals, the next steps will concern
- the choice of the extraction technique
- the evaluation of the performances of the method.
HORIZONTAL Factsheet
Pharmaceuticals
version: 2/12/2016
Placement of PHARMACEUTICALS method in overall structure HORIZONTAL
SLUDGE, SOIL, TREATED BIOWASTE AND RELATED
WASTES
SAMPLING
IN-SITU ,TRANSPORT, STORAGE
SAMPLE PRETREATMENT - INORG
INORGANIC
CONSTITUENTS
PHYSICAL
PROPERTIES
SAMPLE PRETREATMENT - ORG & BIOL
LEACHING
ORGANIC
PARAMETERS
BIOLOGICAL
PARAMETERS
SAMPLE PRETREATMENT
- HYG
HYGIENIC
PARAMETERS
PAH
pH
Bulk density
Characterisation
leaching tests
Impurities (e.g
glass, plastic)
E. Coli
Stability (bio)
Salmonella
Germinating
weed seeds
Clostridium
Phytotoxicity
Enterococci
AOX
Electrical
conductivity
Dry matter
Compliance
leaching tests
PCB
Organic matter*
Solidity
LAS, NP,NPE
Nutrients N, P,
K*
Thixotropic
behaviour
DEPH, DBP
Trace elements
solid *
Trace elements
determination*
Piling
behaviour
Helminth ova
BFR
Flowability
Rapid methods
PCCD/PCDF
Soluble P
Pharmaceuticals
Virusses and
bacteriophages
Plant
Pathogens
Position of PHARMACEUTICALS method in the sequence of steps from sampling to
reporting
Sampling plan
Taking of sample
Transport & storage
Preparation of test portion
Extraction/ Leaching
Pre-treatment
Detection & Quantification, Enumeration
Summary reports
1)Sample conservation, storage and transport are issues that generally are covered in as the final step in sampling standards
2) Preparation of the test portion from a laboratory sample is sometimes part of the next step (digestion or analysis preparation) or can
be covered in a separate standard
3) Summary of test results is a concise summary of the relevant data for the end-user, which can be merged in an overall test report
covering all aspects relevant for the given situation.
4) After defining sampling strategy based on the question to be answered either one of the sampling standards will generally apply. All
the following steps will be the same for either route.
5) It is at present not clear where extraction of organic parameters begins and pre-treatment ends. It seems that pre-treatment now includes
the extraction step.
Major issues of discussion
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HORIZONTAL Factsheet
Pharmaceuticals
version: 2/12/2016