MERCK Analytix Reporter ISSUE 6 | 2019

Significance of the topic

In today’s fast‐paced analytical laboratories, streamlined methods, fully traceable reference materials, and digital data transfer are crucial to ensure both efficiency and compliance across industries from pharmaceuticals to food safety and petrochemicals.

Aims and study overview

This issue highlights a range of recent innovations and products designed to maximize data integrity, speed up analyses, and broaden the scope of detectable analytes. Key topics include:

• Digitalization of titration workflows with RFID‐tagged reagents and SmartChemicals for error‐free data transfer.
• Development of proficiency testing materials for quantitative NMR (qNMR) to demonstrate laboratory competence.
• High‐speed monoclonal antibody titer analysis using silica monolithic columns functionalized with protein A.
• Certified impurity solution mixtures for rapid and accurate pharmaceutical impurity testing.
• A new set of extractables and leachables reference standards to support identification and quantification in packaging studies.
• Implementation of the USP Famciclovir tablet monograph method on Purospher™ STAR RP-8 columns with UV detection.
• QuEChERS extraction and novel dual‐layer SPE cleanup for pesticide residue analysis in ginger using LC-MS/MS and GC-MS/MS.
• HPTLC fingerprinting and a new Stevia extract reference material for rapid quality control of steviol glycosides.
• Ion chromatography applications for sugar profiling in foods and levoglucosan detection in environmental aerosols.
• Expanded food matrix CRMs certified for elemental content and stable isotope ratios to support routine food authenticity tests.
• New sulfur CRMs for calibration and verification in petroleum product testing under stringent fuel standards.

Methodology and instrumentation

A variety of advanced techniques underpin these innovations, including:

• RFID‐enabled titration using METTLER TOLEDO titrators and SmartChemicals for wireless reagent data transfer.
• Quantitative 1H NMR with certified reference materials and a quick‐turn proficiency testing portal for global laboratories.
• Affinity chromatography on wide‐pore silica monoliths with dynamic protein A immobilization for sub‐two‐minute mAb separations.
• HPLC and UPLC methods using C8, C18 and HPTLC plates, with UV, PAD and MS detection modes.
• SPE and dSPE cleanups including the Supelclean™ Ultra cartridges combining PSA, C18, graphitized carbon and Z-Sep for botanical and spice matrices.
• GC-MS/MS and LC-MS/MS for pesticide and leachable analyses with matrix-matched calibration curves.
• Ion chromatography with pulsed amperometric detection for mono- and disaccharide profiling in complex samples.
• Accredited workflows for CRM production and stability testing under ISO 17025 and ISO 17034 standards.

Main results and discussion

• SmartChemicals eliminated manual data entry in titration, reducing transcription errors and saving lab time.
• qNMR proficiency materials enabled rapid, traceable performance evaluation with uncertainties below 0.2%.
• Silica monolith columns modified with rProtein A delivered robust mAb capture‐elution in under one minute, with CVs <1%.
• Pharmaceutical impurity mixes in one‐ampoule solutions simplified daily QC, with recoveries of major impurities within 70–120%.
• New extractables and leachables CRMs offered NIST SRM‐traceable purity for over 100 challenging compounds.
• The USP Famciclovir HPLC method achieved RSDs <0.5% and resolution >1.2 on Purospher™ STAR RP-8.
• QuEChERS plus Ultra 2400 SPE cleanup in ginger powder removed >20% of GC background and yielded average pesticide recoveries of 82%.
• HPTLC fingerprints of steviol glycosides allowed qualitative matching of Rebaudiosides A–D, stevioside and minor components in new Stevia extract CRM.
• IC analysis provided direct sugar profiles in apple juice and lactose checks in “lactose-free” milk with no complex extraction.
• Expanded food matrix CRMs certified for CHNS and δ13C/15N/34S ratios now support authentication tests.
• Sulfur CRMs in mineral oils and fuels cover 0–5.0000% S, fully traceable and accredited for ASTM/IP methods.

Benefits and practical applications

• Fully digitalized titration runs bolster data integrity and speed.
• qNMR PT materials support ISO 17025 lab accreditation.
• Fast mAb assays enhance bioprocess monitoring and QC.
• Impurity solution concentrates save weighing and potential errors.
• Comprehensive E&L standards accelerate toxicological profiling.
• Standardized pharmaceutical monographs ensure regulatory compliance.
• Improved sample cleanup extends method robustness for complex matrices.
• HPTLC traceability aids rapid identity tests in herbal supplements.
• IC sugar analysis streamlines nutritional labeling and environmental tracing.
• Accredited food and fuel CRMs underpin reliable, comparable measurements in routine and forensic labs.

Future trends and opportunities

• Extension of SmartChemicals and RFID‐based reagents to other analytical platforms.
• Growing adoption of quick‐turn proficiency studies across diverse techniques.
• Development of broader monolithic supports for larger biomolecules.
• Expansion of multi‐analyte CRM mixes for emerging contaminants.
• Integration of HPTLC and mass spectrometric imaging for advanced botanical fingerprinting.
• Enhanced inline sample preparation systems to further automate workflows.
• Adoption of stable isotope ratio analysis for food provenance verification.
• New certified reference materials for next‐generation fuels with ultra‐low or specialty heteroatom profiles.

Conclusion

Innovations in reagents, materials, and digital integration are driving a new era of high‐speed, high‐confidence analyses across pharmaceutical, food, environmental, and petrochemical sectors. The combination of SmartChemicals, accredited CRMs, advanced separation media, and robust workflows ensures laboratories can meet stringent quality requirements while maximizing throughput and traceability.

References

1. Straub‐Jubb, B. et al. Titration 4.0: SmartChemicals for data integrity. Analytix Reporter 6 (2019).
2. Duhon, J.; Breitruck, K. Quality Assurance in qNMR: Proficiency Testing. Analytix Reporter 6 (2019).
3. Kupfer, T. et al. Silica Monoliths for Fast mAb Analysis. Analytix Reporter 6 (2019).
4. Hauser, N. Pharmaceutical Impurity Solution Mixtures. Analytix Reporter 6 (2019).
5. Nold, M. New Reference Materials for Extractables & Leachables. Analytix Reporter 6 (2019).
6. Shinde, S. Famciclovir Tablets USP Monograph HPLC Method. Analytix Reporter 6 (2019).
7. Stenerson, K.K. QuEChERS and Dual‐Layer SPE for Ginger Pesticides. Analytix Reporter 6 (2019).
8. Frommenwiler, D.; Broszat, M. Steviol Glycoside Fingerprinting by HPTLC. Analytix Reporter 6 (2019).
9. Emmenegger, C. Ion Chromatography for Sugars in Food & Air. Analytix Reporter 6 (2019).
10. Nold, M. New Food Matrix & Isotope Ratio CRMs. Analytix Reporter 6 (2019).
11. Withers, E.; Nold, M. New Sulfur CRMs for Petrochemical Testing. Analytix Reporter 6 (2019).