Automação de SPE utilizando sistema robótico Triplus RSH autosampler

Nova Analitica

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ITSP Introduction

The heart of the ITSP system is a patented cartridge containing customer-defined filter and/or SPE media.

ITSP is Instrument Top Sample Prep

On a Triplus RSH autosampler the ITSP cartridge can be moved over trays or vials to facilitate sample

clean-up through JIT automated filtration or SPE (Solid Phase Extraction).

ITSP Introduction

JIT – Just In Time – prep the next sample while the previous sample is being analyzed, which means no analyte degradation between first and last samples,

as can be seen in batch processes using a liquid handler!

ITSP Cartridge Components

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Triplus RSH Lower Needle Guide

(modified )

Triplus RSH Syringe Needle

SPE Sorbent or Filter Media

The small inner diameter of ITSP needle guide - reduces volume to improve efficiency, - maintains vertical position of ITSP cartridge during transport, and is - color coded for different sorbents.

Needle Guide

The cartridge septum grips the needle to allow the Triplus to transport the ITSP cartridge.

Septum

Media Cup

8mm Crimp Seal

The crown of the ITSP cartridge seal mates with the nipple on the Triplus RSH lower needle guide to center the needle in the cartridge.

A funnel cone beneath the septa guides the syringe needle into the central bore of the cartridge.

A dispersion cone beneath the syringe needle tip disperses the solvent/sample over the sorbent bed.

The needle penetration for ITSP tray types is set by default to 20mm: • This allows the tip of the needle

to be positioned at the top of the dispersion cone above the sorbent bed.

• Longer penetration may cause the needle to core the sorbent bed.

• Shorter penetration may not keep the cartridge aligned properly in a vertical orientation during transport.

2cm

ITSP Cartridge Details

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ITSP Cartridge Configurations

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• ITSP SPE cartridges are available in a very large variety of sorbents. • There are two bedmass sizes:

– nominal 10mg (standard) and nominal 30mg (large). • Multiple sorbent manufacturers. • All standard sorbent phases

• Reverse phase, • Normal phase, • Ion exchange, • Copolymeric (mixed-mode), • “Special” configurations,

e.g. QuEChERS blend, coconut charcoal, and • Custom configurations – tell us what you want.

• Typical solvent and sample volumes are in the 100μL range using sorbent bed masses from 10 mg to 25 mg.

How ITSP Performs SPE

The analytical syringe replaces the column sample reservoir above the sorbent bed as found in manual SPE cartridge formats.

The needle penetrates the septum and creates a seal so that the sample or solvent is forced through the sorbent bed by positive pressure when the plunger is depressed.

Solvents and sample are forced through the SPE sorbent bed by the analytical syringe plunger.

The sample is eluted into a collection plate and then injected into the LC injection valve.

Unlike manual SPE methods which require a vacuum manifold, ITSP solvent and sample flow rates can be precisely controlled with the syringe plunger.

How ITSP Performs SPE

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ITSP Hardware

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ITSP Prep / Waste Station • Conditioning

• Loading Sample • Washing

ITSP Prep / Waste Station

ITSP Hardware

ITSP Tray Type VT54ITSP • Eluting step

ITSP Tray Type VT54ITSP

ITSP Hardware

Triplus RSH

Holder station

Vortexer

Wash station

Solvent station

Tray station

ITSP Applications

• Clinical/Forensic – • Many analytes (drugs) from many matrices (urine, blood, hair, saliva):

• Pain management drugs from patient urine samples • Vitamin D from patient blood plasma samples (using C8 or C18) [RP], • Forensic drugs of abuse from case urine or corpse blood samples • Steroids from blood plasma or serum (using C8) [RP], and • Immunosuppressants from blood plasma or serum (using C8) [RP].

• Environmental/Food and Beverage – • Pesticide residues from food QuEChERS extract clean-up (proprietary blend), or • Contaminants from beverage or drinking water (coconut charcoal).

• Pharmaceuticals – • Small sample volume – “micro-sampling” (2-5µL) – automated SPE of pharma COI’s

(Compounds Of Interest) from biological/botanical sample matrices (C8 or C18) [RP].

• Emerging Markets – • Legalized marijuana (both potency of, and contaminants in, THC).

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ITSP Applications

Why should a lab consider ITSP?

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ITSP can provide many benefits:

• Improve quality of chromatography by improving peak shape and reducing interferences,

• Extend LC column life by more than 1,000% over dilute-and-shoot methods,

• Reduce risk of carry-over,

• Increase lab throughput,

• Reduce costs of capital equipment,

• Reduce cost of solvent acquisition and hazardous waste disposal – in some cases by 90% or more (ITSP is green),

• Utilize valuable analytical chemist’s time for data analysis instead of taking up time for sample prep, and

• ITSP uses standard SPE protocols, except miniaturized and automated.