Purity confirmation
The price we quote depends on the purity of the product to be guaranteed.
The higher the guaranteed purity, the higher the price.
We usually quote a purity of 95% area ratio if specific purity is not shown from the customer.
・Purity as stated on the quotation is goal.In the case of a small scale of less than 100 mg, if purification is not particularly difficult with some exceptions, such as stability problems, mixed impurities that are difficult to separate such as isomers, etc., we usually submit more than 98-99%.
On the other hand, if it is difficult to achieve the targeted purity due to difficulty in removing impurities, the product will be delivered with impurities included, and the full amount will be invoiced and settled, and additional purification will be discussed separately.
Unless otherwise stated in the remarks column, purity is judged by the area ratio of the chromatogram obtained under the analysis conditions set by us using our analysis equipment.
Please note that it is not absolute purity, content, mole%, or weight%.
・If it is found that a high-purity product cannot be obtained due to the stability of the objective substance, the product will be submitted with less than the targeted purity, and the full amount will be settled. Stability tests and establishment of purification conditions under stable conditions will be discussed separately.
Please also refer here.
In some cases, we may determine that it is difficult to purify due to stability and submit the product unpurified.
We determine the purity as follows.
- Compounds with strong UV absorption: area ratio in HPLC UV chromatogram. Maximum absorption wavelength of the objective substance is selected.
- Compounds with no UV absorption or volatility: area ratio by chromatogram with HPLC ELSD detector
- Volatile compounds without UV absorption: area ratio in GC or GC/MS (TIC) chromatogram
- Compounds for which no signal is detected by HPLC, GC, or LC/MS: Determined by TLC image data showing one spot.
- Compounds that decompose during analysis, making it difficult to measure the purity of the compound itself: Analyze some modified derivative of the compound.
・Please note that in both cases, it refers to the area ratio of each peak in the HPLC analysis chromatogram or the spot visual inspectionof the TLC analysis, not the content or the purity in the exact sense.
Content measurement, absolute purity measurement, warranty, etc. can be handled by us, but are subject to separate consultation.
・If you would like to request specifications that exceed those listed in the quotation after placing the order, we will respond separately at an additional cost after the contract is completed and invoiced.
If a lot of product that has already met the target purity stated in the quotation is requested to be re-refined for the purpose of further purity improvement, it will be handled at an additional cost only if we judge that it is technically possible.
・The properties of compounds are not guaranteed unless otherwise stated in the remarks section, and may be delivered in syrup or liquid form even if the literature description is solid or powder.In many cases, crystallization can be achieved by detailed studies such as heating, cooling, prolonged decompression treatment, and ultrasonic treatment, but this may require time and effort, and will be handled at an additional cost.
・In the case of liquids or syrups, it may be difficult to completely remove the solvent by vacuum drying, and a few percent may remain.
・Coloration may occur due to minute amounts of impurities. Specifications are based solely on the chromatogram purity listed in the certificate of analysis.
The same applies to odors. Deodorization, decolorization, and other treatments are available at an additional cost.
・We usually select a purification method that does not contain inorganic substances, but it may be difficult to remove them, especially for highly polar compounds.
If you do not want a small amount of inorganic material mixed in, please let us know before placing an order.
・In the case of repeat synthesis, we do not guarantee the same quality as the previous time in principle.
This service is available only if you inform us before placing an order that you require a guarantee that the quality and properties of the product are equivalent to those of the previous product, and that you require a report of the analysis data in comparison with the previous product.
The price and delivery time will vary greatly depending on the level of warranty required and the nature of the work
・Comparative analysis with other companies' products and commercial products is also handled in the same way as above.
・Optical purity: For final products and intermediates including asymmetric synthesis processes, please consult with us individually.
In the case of synthesis using commercially available optically active raw materials, unless otherwise stated in the remarks column of the quotation, we will omit any confirmation of the optical purity of the raw materials, intermediates, and submitted products, without considering the possibility of isomer contamination of the raw materials or racemization during synthesis, and the optical purity will not be guaranteed.
If the procedure is as described in the paper, the possibility of racemization is considered to be low, but we will report and consult with you if there is any concern about racemization in our consideration.。
If you need to confirm the optical purity of commercial raw materials, finished products, or intermediates, please consult or request a specialized analysis company.
It may be necessary for us to submit analysis samples, so please be sure to let us know at the time of inquiry. We do not accept requests made after the order has been placed.
In the chiral column method, it is not enough to show that there is a single peak.
The optical purity can only be determined when the isomers are synthesized separately using the same synthetic method and the analytical conditions are established so that the S and R isomers show separate peaks.
In the derivatization method, two types of diastereomers are created by reacting with both the R and S forms of the chiral reagent that lead to diastereomers, and if HPLC analysis conditions can be found that allow the separation of each, optical purity can be calculated, but in many cases the separation of each isomer is difficult or impossible, so it is difficult to offer a success reward.
Purification of commercially available raw materials, intermediates, or finished products to confirm or improve optical purity is available on an individual basis at an additional cost.
Recrystallization, chiral column method, derivatization method, etc. are possible, but all of them are very complicated and require a long time.
・In the case of raw materials that may contain isomers, whether supplied by the customer or arranged by us, generation of impurities caused by the raw materials are not guaranteed.
If there is a problem with the purity of the submitted product due to isomers contained in the raw materials, and resynthesis is required, we will consult with you for a separate fee.
・If there is a possibility that alpha-anomer and beta-anomer are generated in the synthesis of saccharides, we will trust the description in the reference and omit detailed structural analysis. Alpha/beta ratio may be possible by detailed structural analysis, but please consult with us separately.
・We are not responsible for the performance of the compounds, unless otherwise stated in the remarks section of the quotation.Please do not refuse acceptance for the following reasons. Examples are given below, but are not limited to.
I tried to perform a reaction using the delivered product, but it did not work. →We will conduct a model experiment using a part of the synthesized product if you contact us before placing an order.
We tried to polymerize using the monomer delivered from our company, but it did not polymerize well.
The solubility is not as good as I expected.
Dissolvability, color and shape of the crystals are different from what you expected or expected.
The expected activity is not observed.
However, if the product is found to be defective before acceptance inspection, or if the chromatogram reveals the presence of impurities that cannot be detected, we will work on re-purification or synthesis of an alternative product, so please consult with us separately.
・If you have any questions about the purity of the deliverables after we have received your acceptance notice,we will address them immediately.
If the results show that there is no problem with the purity of the delivered product, but that the decrease in purity is due to decomposition during storage or manipulation during use, we may charge the full amount or part of the cost of our confirmation experiment separately.
About content
We do not guarantee the content or measure the content because of the cost and effort involved.The following conditions may apply only if we consult with you before placing an order.
・Only compounds that can be confirmed by q-NMR are supported.
・Synthesis and content assurance are handled as separate requests. The synthesis cost is invoiced upon completion of the synthesis, and the content measurement is handled on a separate request.
・As for the content guarantee, only when it is technically possible, re-refining is available at an extra cost.
・Analysis using a portion of the submitted data. Recovery and refining costs are not included.
About salt
For acidic or basic compounds, unless otherwise stated in the remarks column, we will first consider submitting them in free form, but for the sake of stability and ease of purification, we may submit them in some form of salt for convenience in purification.
In addition, there are cases where the actual delivery differs from the quotation (free body → submitted as salt, change of counter ion, etc.).
If you wish to specify or change the type of salt after placing an order, we will do our best to accommodate your request.
(1)We will finish with the actual product before processing, settle the bill, and make another request.
(2)There is a possibility of significant weight loss due to additional work. Additional synthesis for the shortage will be discussed separately.
(3)Disassembly or loss of purity due to additional work is not guaranteed.
If the customer wishes to have the product re-purified to remove the degradation products, this will be discussed at an additional cost.
Please also read our thoughts and actions regarding the stability of the objective substance.
About LC/MS adduct ions
・We often use LC/MS data as a means of confirming the structure and purity of synthetic products.
A variety of additional ions are detected depending on the objective substance or impurity, and the detection of multiple additional ions at targeted peak positions and changes in MS spectra due to buffer changes provide strong evidence to support the identity of the analyte.
If you find an unknown signal in the MS spectrum of your LC/MS data, please refer to the following list first.
| ESI positive | detected ions | Notes |
|---|---|---|
| [M+H]+ | M+1 | amines |
| [M+NH4]+ | M+18 | |
| [M+Na]+ | M+23 | |
| [M+K]+ | M+39 | |
| [M+H+NEt3]+ | M+102 | in triethylammonium buffer |
| [M+H+CH3CN]+ | M+42 | |
| [M+NH4+CH3CN]+ | M+59 | |
| [M+Na+CH3CN]+ | M+64 | phenol origoethoxylates |
| [2M+H]+ | 2M+1 | |
| [2M+NH4]+ | 2M+18 | |
| [1/2M+NH4]+ | 1/2M+18 | PEG analogs |
| [1/nM+NH4]+ | 1/2M+18 | high MW PEG analogs |
| [2M+Na]+ | 2M+23 | |
| [M+2H]2+ | M+2 | |
| [M+2Na]2+ | M+46 | |
| [M]+ | M | quaternary ammonium |
| ESI negative | detected ions | Notes |
| [M-H]- | M-1 | carboxylic acid |
| [M+Cl]- | M+35, M+37 | |
| [M+HCOO]- | M+45 | in formic acid buffer |
| [M+CH3COO]- | M+59 | in acetic acid buffer |
| [M+CF3COO]- | M+113 | in TFA buffer |
| [2M-H]- | 2M-1 | |
| [1/2M-H]- | 1/2M-1 | |
| [2M+HCOO]- | 2M+45 | in formic acid buffer |
