Mass Spectrometry & Spectroscopy
Compliance, CRMs and Accreditation in Spectroscopy – A Supplier’s Perspective Nathan Hulme & John Hammond, Starna Scientifi c Ltd. Email:
sales@starna.com
Since the 1970s, Instrument Qualifi cation in testing laboratories has become an essential part of regulatory compliance. This brief history describes how regulators and commercial suppliers have met the demand for reliable reference materials to facilitate compliance
In the beginning
Any respectable analytical laboratory strives to achieve quality results, recognising that to do so, its instrumentation must be working correctly and be qualifi ed by regular performance checks. Prior to the 1970s, most laboratories used home-made test solutions or proprietary test materials to perform these checks. Alternatively they relied on the instrument manufacturers’ service organisation to calibrate their instruments as part of routine maintenance. Manufacturers like Optiglass (now Starna Scientifi c) supplied calibration standards such as rare earth glass fi lters for ‘Wavelength’, and neutral density fi lters and rare earth wavelength references primarily for ‘Absorbance’ to instrument manufacturers and some end users; whilst Starna supplied sealed liquid references such as potassium dichromate, lithium carbonate, holmium perchlorate and benzene vapour. In the meantime, the only available references with internationally recognised and certifi ed calibration values were those from National Measurement Institutes (NMIs) such as the National Institute of Standards and Technology (NIST) in the United States, whose products were trademarked as Standard Reference Materials (SRMs).
Up until 1975 analytical results had been very much taken on trust, but then allegations were made, and subsequently proven against two major testing laboratories in the US, that results submitted during preclinical drug safety testing were seriously fl awed and in some cases, had been deliberately falsifi ed. This led to the publication, in 1976, and subsequent entry into US law of Good Laboratory Practice (GLP) [1], a code requiring non- clinical testing laboratories to implement formal quality control procedures. These included the requirement for laboratories to qualify their instrumentation using properly characterised test and control materials. GLP has since been adopted (in 1981) in the Organization for Economic Corporation and Development (OECD) guidelines [2], it is also enshrined in EU law [3], alongside all the other GxP (where x=m, etc.) related standards used in the pharmaceutical industry. GLP specifi cally has expanded out of the pharmaceutical sphere in to most areas of laboratory analysis,
notably into the food and environmental sectors. Instrument qualifi cation is now mandatory in any laboratory working in a regulated environment – and represents signifi cant benefi t to those that are not.
Instrument Qualifi cation
Analytical instrument qualifi cation is conventionally described as a four-step process: Design Qualifi cation (DQ), Installation Qualifi cation (IQ), Operational Qualifi cation (OQ) and Performance Qualifi cation (PQ) [4]. In simple terms, DQ and IQ are usually performed by the instrument supplier, OQ demonstrates that the instrument meets its published performance specifi cation, and PQ verifi es the fi tness for purpose of the instrument under the actual conditions of use. In a routine situation, only PQ will need to be performed on a regular basis, whereas OQ is done less frequently, usually after maintenance or repair have been carried out on the instrument. All major pharmacopoeias and regulatory authorities publish standards specifying the qualifi cation tests required for compliance, which must be conducted using recognised test materials or standards. While it is perfectly possible for laboratories to prepare their own test solutions, such procedures have several attendant risks, such that it is now widely accepted to be more convenient, cost effective and less prone to error to purchase certifi ed reference materials from a suitably accredited supplier. Indeed, General Chapter <857> of the US Pharmacopeia [5] states: “Wherever possible…. certifi ed reference materials (CRMs) are to be used in preference to laboratory-prepared solutions.”
From NMIs into the private sector
The GLP requirement for instrument test materials to be properly characterised led to a surge in the demand for standards from the NMIs, exceeding their production capacity. NIST therefore decided to investigate whether the skills to be found in private sector companies like Starna Scientifi c could be harnessed to the production of reference material to meet the demand. Indeed,
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