- Samples are analyzed as soon as possible upon receipt. If a more urgent timeline is needed please contact us at sales@axispharm.com.
- For each submitted sample and blank solutions, three individual data points (absolute intensity) are recorded and averaged. The averaged intensities are used in conjunction with the linear regression data from the calibration curves to calculate the concentration of the element in solution.
- Users will be contacted by email once samples have been analyzed. All results will be submitted by email via PDF.
- Within the results report, all pertinent instrumental conditions, calibration curves and calculated concentrations in samples are provided.
- Raw data and Electronic copies of the results are archived. If needed, please contact the lab staff at sales@axispharm.com.
- All samples are refrigerated at 0-4 °C for a maximum of one month. Please ensure to retrieve your samples as soon as possible. If you require alternative sample storage conditions, please let the lab technician know and ensure to include such information in the sample submission form.
ESI/APCI-MS Analysis
Sample must be prepared at ~ 0.1-1.0 mg/ml with a sample volume of ~0.05-0.1 ml using MeOH, ACN, or H2O. Avoid salts, DMSO and DMF, buffers, stabilizers and detergents.
GC-MS Analysis
Sample concentrations should be ~0.1-0.5 mg/ml. NEVER exceed a concentration of 1.0 mg/ml, if you do you can damage the GC column or the MS components.
Samples must be prepared in most volatile organic solvents, preferably acetone, methanol, hexane, aromatics, and alkanes. Less preferable are halogenated solvents (e.g. chloroform, methylene chloride, etc.) and ethers (e.g. diethylether, THF). DO NOT use water, DMF, or DMSO as a solvent. Place your sample in a GC-MS specified sample vial with the correct septum and cap, i.e. Agilent Part Number 5182-0714 (Pack of 100 screw top vials) and Agilent Part Number 5182-0717 (Pack of 100 Blue screw caps and PTFE/red rubber septas). Sample must fill at least half of the vial volume.
High Resolution MS Analysis
HR-ESI/APCI-MS analysis: Please provide at least 10 ug neat compound or prepare the sample at ~ 0.1-1.0 mg/ml with a volume of ~0.05-0.1 ml using MeOH, ACN, H2O, Acetone, or DCM. Avoid salts, DMSO and DMF, buffers, stabilizers and detergents.
ICP-MS Analysis
- All samples must be supplied in clearly labelled and closed plastic containers.
- For quantitative analyses, please submit the following in addition to your samples: Calibration solutions (five separation solutions prepared by serial dilution) that contain the target elements with following concentrations: 1000 ppb, 100 ppb, 10 ppb, 1 ppb and 0.1 ppb
- All sample containers should be cleaned beforehand by soaking in 2% HNO3 (aq) overnight, then rinsed with ultrapure water (MilliQ preferred) and then dried in a clean air fume hood.
- All samples need to be submitted as either a liquid that can be analyzed by ICP-MS directly (e.g., water samples) or as dissolved samples diluted in weak mineral acid(s).
- Please use trace-metal grade mineral acids for all samples and calibration solutions.
- Please ensure that the same matrix (i.e., mineral acid) as used in the sample is used in the calibration solutions and blank solutions.
- For all samples, please make note of the sample weights and dilution factors so that the final concentrations of the targeted elements in your samples can be calculated.
- It is vitally important that the submitted samples are solutions that DO NOT contain any dissolved solids (either original non-dissolved sample or salt precipitates). Samples should be filtered (at least 0.45 micron) and acidified as soon as they are collected to ensure metals are retained in solution.
- The preferred concentration of elements for analysis in solution is 10-100 ppb (parts per billion by weight; e.g., ng/g) for trace elements or 1 ppm (part per million by weight; e.g., µg/g) for major elements (i.e., Si, Ti, Al, Fe, Mg, Mn, Ca, Na, K, P).
- Sample consumption during analysis is typically between 5-10 mL. To ensure sufficient amount of sample is available, please submit 10 mL samples.
HPIC Analysis
- All samples must be supplied in clearly labelled and closed plastic containers.
- Samples should be filtered (at least 0.45 micron).
- Sample consumption during analysis is typically between 5-10 mL. To ensure sufficient amount of sample is available, please submit 10 mL samples.
MALDI-TOFMS Analysis
Certain requirements need to be met in order to obtain good quality MALDI-TOFMS data:
1. Use only volatile solvents/buffers such as MeOH, H2O, CH3CN etc. Avoid using non-volatile agents such as salts (e.g. NaCl, CaCl2, KH2PO4), detergents (e.g. Triton, SDS), Urea, Guanidinium salts, and DMSO, DMF, and Glycerol.
2. If the above-mentioned components can’t be avoided, then purify. dialysis, ZipTips (Millipore Corporation), and reversed phase HPLC are good purification methods (use volatile solvents and buffers e.g. 50% ACN in water with 0.1% v/v trifluoracetic acid).
3. Sample with typical concentration of 5–100 µM and minimum volume of 2 uL is required. The total amount of sample needed for MALDI analysis is related to their molecular weight. For small molecular weight (1,000 or less) the minimum amount needed for analysis is 16 picomoles/microliter. The minimum for molecular weight 20,000 or less is 60 picomoles/microliter, and for 66,000 molecular weight the minimum amount needed for analysis is 160 picomoles/microliter.
4. Helpful information include: structure, sequence, molecular weight, type of compound, chemical reactivity, pH, sample amount/concentration, description of purification/isolation with focus on relative agents/solvents, suitable solvents, hazardous properties etc.