TECHNIQUES Sample Preparation Digestion techniques Chromatography - - PDF document

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BecA‐ILRI Hub Laboratory Management and Equipment Operations (LMEO) workshop‐ RUBONA, Rwanda

TOPIC: LABORATORY INSTRUMENTATION

DATE DATES: 18

18th

th June 201

June 2015 Tom O Tom Ouma ma

LABORATORY PROCESS

Data

Data Analysis Decision Making/Recom

Testing

Sample Preparation Instrument

Scientist

Method Development Sample

VALUE OF LABORATORY EQUIPMENT

1. The value of each laboratory equipment is mainly measured based

• n its capability to provide data which is reliable, consistent, timely

and affordable. 2. It is critical that prior to acquiring any equipment, a proper need assessment should be carried out to ascertain the demand and technical requirements. 3. It is also important that one considers the long term value addition/benefits against the cost. 4. It is advisable that the user/manager consult with the equipment distributors/manufacturers in order to know the current technology available and their capabilities. 5. Networking with other labs in the same category is highly encouraged. 6. Resource mobilization is important prior to procurement. 7. Competent technical evaluation should be carried out on all offers.

ASPECTS OF INSTRUMENTATION

For effective laboratory instrumentation to be achieved, the following aspects should be met; 1. The laboratory management system should be in place to guide the acquisition(including supplier audits), utilization, maintenance & disposal of the instruments. 2. The equipment must be properly installed. 3. The equipment must be qualified(IQ ,OQ & PQ) prior to use. 4. Maintenance service contract is highly recommended. 5. Calibration schedule should be in place where necessary. 6. Records on complaints, investigation, corrective action & internal audits should be available throughout shelf-life. 7. Should be capable of enhancing high levels of confidentiality/user level controls & Audit trail features. 8. There should be effective resource utilization programs. 9. There should be a master list of all the equipment and their status update.

MAJOR STEPS IN SAMPLE TESTING

Sample Preparation

SPE LLE QuEChERS Digestion -Multiwave

Sample Seperation

LC GC

Compound Detection & Quantification

PDA UV MS, MS/MS,

TECHNIQUES

Digestion techniques – Multiwave digestor, Hydrotherm, Soxtherm(fat & Lipids, Dumatherm(Protein & Nitrogen, Kjeldahltherm (metals, COD, Cyanide) Chromatography AAS & ICP (Elemental) FTIR Spectro Raman Spectro UV-Vis XRD/EDX/XRF NIR Polarimetry Refractometry

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Application

• Chromatographic technique is widely applied in

most environmental, drugs and food testing with HPLC and GC being the commonly used.

• HPLC –Carbomates, pesticides, PAHs and

explossives.

• GC- Pesticides, Herbicides, VOCs, SVOs and

PAHs (Polinuclear Aromatic Hydrocarbons.

Trace Level Residue Analysis

• Many compounds like pesticides have been

discontinued due to health & environmental risks. Their continued use has left heavy contamination & need of remediation.

• PAHs are a class of persistent organic pollutants.
• Need for:

1.

Plant & Food protection.

2.

Food chain safety.

3.

Environmental risk assessment.

4.

Crisis response.

5.

Economic gain.

MULTI-RESIDURE TESTING IN FOOD

QuEChERS

roQ Quechers

roQ quechers Kits (Phenomenex).pdf

11

SHIMADZU LC-MSMS

Sprayer Qarray Skimmer Octopole 1 Desolvation Line UFsweeperTM Collision Cell Q3 Detector Octopole 2 Q1 Q1 Pre‐rod Q3 Pre‐rod Q1 Post‐rod 1st Vacuum chamber: 100 to 200 Pa 2nd : 5 Pa 3rd : 0.1 Pa 4th : 3 x 10‐3 Pa Atmospheric Pressure

4 Stage Differential Pumping System by a Triple Inlets TMP and a RP

40 L/S 260 L/S 210 L/S

RP

12

Requirements for Triple Quads

Sensitivity Reproducibility Speed Robustness Usability Affordable Price

Pharmaceutical Life Science Chemistry Molecular Imaging Nano Technology Food Safety Electronics New Energy Environmental Forensic

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MULTI-RESIDURE METHOD

Neat std mix 138 compounds on LC-MS/MS 8040

72 =LC-MS/MS 66 =GC-MS/MS LC/MS/MS LOQ <10ppb

72 (100%)

GC/MS/MS LOQ<10ppb

47 (71%), >10ppb 6(9%)

80% compounds reffered

to GC/MS/MS were able to be measured by LC/MS/MS

APPLICATION Mycotoxins

SHIMADZU Method packages provide pre‐

• ptimized MRM and HPLC conditions

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Compound ID

3.0 3.5 4.0 4.5 5.0 5.5 min 0.0 1.0 2.0 3.0 4.0 5.0 6.0 (x100,000) 200 250 300 m/z 0.0 1.0 2.0

• Inten. (x100,000)

235 263 308 221

Injection Blood, Urine, Organ QuEChERS Spectrum is acquired at same time

N N NCH3 CH3 O CH3 C H3

Zolpidem MS/MS spectrum (Product Ion Scan) Compound ID by Library search Data Output Chromatogram (MRM)

LCMS-8060

NEXERA SERIES

Nexera TQ and Nexera SQ

• ffers ultra-fast LC/MS analysis by

combination of Nexera X2 and UF-MS.

Nexera Method Scouting

• ffers comprehensive method

development by 96 combinations

Nexera MP LC/MS

frontend HPLC for high throughput analysis of multiple samples.

Nexera SR

features superior sensitivity, sensitivity and stability.

Nexera Quaternary

is flexible quaternary gradient system.

INTEGRATED HPLC SYSTEM Prominence-i & Nexera-i, Series

ESTEC LTD

Educational Scientific & Technical Company (ESTEC) is a leading distributor of quality analytical instruments within East Africa region and has been in operation for the last 37 years. During this period, ESTEC has developed into a dependable partner supporting various industries mainly Pharmaceuticals, Research, Beverages, Regulatory, Petroleum, Food, Environmental and educational laboratories. Estec has won the confidence of leading global brands from Europe, Asia and USA by being appointed the sole dealer for Shimadzu(Japan), Anton-paar(Austria), Gerhardt(Germany), Phenomenex(USA) among others. At Estec we nurture and cultivate a culture of a serving relationship with each customer and this is why we don’t just deliver, we see you through the equipment life-span. We boast of a strong team of technically skilled, experienced and reliable engineers as well as sales staff capable of installing, training, and servicing your instruments. With Estec, you are in safe hands.

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1. Application Support

• 2. Service Support

BENEFITS

Method packages Residual Pesticides. NIST Libraries for Vet drugs, Pesticides, Forensic drugs. User friendly easy to learn & operate LabSolution software. User Training. Locally available skilled Technical support & Spares. Maintenance Service contract.

KEY AREAS OF SUPPORT

• 1. Environmental Labs.
• 2. Food & Agricultural Labs.
• 3. Pharmaceutical Labs.
• 4. Petroleum Labs.
• 5. Beverage Products.
• 6. Forensic Labs.
• 7. Mining Labs.
• 8. Research & Educational Labs

The End The End

Thank you Thank you for your for your valuab valuable le

• rders &
• rders & listening

listening.

Tom Ouma Tom Ouma

+254- 254-722 990 22 990 99 996 6 info@esteckenya.com