Synthesis Of Lidocaine Lab Report

As of October 2, 2017 there has been a reverified shortage of the Lidocaine Hydrochloride injection. The generic name is Lidocaine where the brand name is Xylocaine. It is a Local Anesthetic and an Antiarrhythmic Agent Class 1b. Xylocaine is used as a local anesthetic by infiltration, epidural or nerve block; and it also used to treat ventricular arrhythmias from myocardial infarction.

Materials. The following chemicals are purchased and used as received. Cadmium oxide (CdO, 99.99 %), and potassium sulfide (K2S, 95 %) are obtained from Strem Chemicals. 1-octadecene (90 %), 3-mercaptopropionic acid (99 %), and α-terpineol (97 %) are purchased from Acros Organics. Selenium powder (Se, 99.99 %), oleic acid (OLAC, 90 %), oleylamine (OLAM, 70 %) and acetic acid (99.7 %) are purchased from Sigma-Aldrich. Toluene (99.9 %), 2-propanol (99.9 %), ethanol (90 %), acetonitrile (99.9 %), and formamide (FA, 99.6 %) are acquired from Fisher Scientific. P25 TiO2 and ethyl cellulose (5 % in toluene and ethanol) are supplied by Evonik Degussa Corporation and TCI, respectively. OLAC, OLAM, and FA are dried using standard procedures.

Although high-performance liquid chromatography (HPLC) analysis is provided by most companies to show that the material is pure, yet, doesn’t really reveal much as the product supplied was purely an incorrect compound.

Lidocaine is one of many anesthetics that block the action potential in a nerve from occurring, therefore preventing any sensation. These anesthetics work by blocking the way cells communicate to each other. When a nerve is in its resting potential it is not “talking” to other cells, and the inside of the membrane is more negative (McCance & Huether, 2014). When the neuron gets stimulated to “talk” to other cells the ion channels open. This allows sodium to pass creating a positive charge inside the membrane. Lidocaine blocks the sodium channels, not allowing the action potential to occur. In return, this decreases or even prevents any feelings in the desired areas. Answering the question, the sodium ion channel is blocked by the lidocaine

The formation of the imine is carried out by adding 0.213 grams of ortho-vallin, the aldehyde, and .150 grams of para toluidine. The solids were grinded until homogenous, one layer is formed. The crystals went from brown to orange liquid layer. The bi-product of imine formation is water, and OH gets protonated and come off during the reaction. Recrystallization is done to get rid of water. Hexane is used as the recrystallization solvent because it is non-polar, like the imine. The mass is 0.3365 grams and the percent yield is 99.6%. There was some product lost on the stirring rod. The IR showed a peak at 2942.40 indicating a methyl group and a peak at 1593.67 and 1614.90

The procedure was carried out as follows in the CHEM2210 Laboratory Manual from page 58 to 59.

Diluted essence (10ml, 100 times diluted) was pipetted into a 100ml separating funnel. 20ml of dichloromethane was added to the diluted essence. The funnel was then shaken vigorously for 2 minutes with gas being release occasionally. The organic phase (lower layer) was released into a 100ml beaker and another 20 ml of dichloromethane was added to the funnel and shaken vigorously for another 2 minutes. The organic phase (lower layer) was again released into the 100 ml beaker. The contents of the funnel were disposed of. The organic phase was then added back into the separating funnel with 40ml of 0.1M sodium hydroxide solution and shaken well for 2 minutes. The organic phase was released and disposed of and the aqueous phase was kept and transferred to a 250ml volumetric flask and the volume was made up with 0.1M sodium hydroxide. Standards were then made using the 50mg/L standard provided and mixing with 0.1M sodium hydroxide to create standards with 1,2,3,4,5 mg/L concentrations. Each solution was run through the UV – Visible spectrometer to find the absorbance and then the concentration.

The final yield for this compound was 0.01 or 1%, mainly because of human errors. Possibly, the starting reactants may have been incorrectly mixed or mixing temperature could have been exceeded. Other plausible error might have been incorrect use of separating funnel or reflux condenser. Overall yield cannot be calculated due to a fact that no other measurements took place during this experiment to help determine the overall yield. To increase the final and overall yields, the starting reagents should be mixed properly, separating funnel should be used with great care and laboratory schedule provided should be followed.

The Abstract is also presented in a coherent manner. It summarizes the objective and the main results (LOD, LOQ, R2 values). It also highlights the advantage of the internal standard used as well as going into detail about the simplified sample preparation and the efficient liquid- extraction step, which all contribute to the method’s development.

Sodium hydroxide solution then added to apply a protocol and the solution was heated at 140 °C for 1 h and at 180 °C for 4 h. The alkaline hydrolysis of Gdcl3 should be carried out in substoichiometric conditions, too.

In the proposed method, the sample solution is dissolved in acetonitrile with (1 mg/mL of an analog of fentanyl (CH2CH2CH2) as an internal standard) so that the sample solution is at a concentration of 0.1mg/mL. 1mL of the acetonitrile solution is placed into a centrifuge with 50mg of 4-DMAP (4-(dimethylamino)-pyridine) and 50microL of HFBA (heptafluorobutyric anhydride). The solution is allowed to react for 1h at 75C, following which 5 mL of isooctane and 1N of aqueous sodium carbonate are added, and then centrifuged. 1 mL of this layer is then diluted using 10 mL isooctane. 5 mL of this dilution is placed in a centrifuge tube and back extracted using 5mL of 1 N sulfuric acid. The solution is then ready to be chromatographed. If the sample solution is adulterated with sugars, prior to dissolving the solution in acetonitrile, dissolve an amount equivalent to .1 mg of fentanyl in

The materials and methodology was followed as per the guidelines given in the lab manual(Ajlouni,2015).

Stock solutions were prepared in isooctane, and then diluted into seven concentration levels, from 1 to 500 µg/L. The stock solution was kept at -18 °C until use.

Upon completion of the experiment, it was calculated that the percentage yield of the crystalline product is approximately 60 %, as shown in the calculations below:

The purpose of the lab was to accurately and efficiently determine the physical and chemical properties of a provided 5.0 grams of Unknown White Compound (UWC), 631r, in order to properly identify and dispose of the UWC. A continuation of the lab was to then synthesize the identified the UWC by using basic laboratory skills and equipment. To identify the UWC, a series of tests were performed, such as the solubility test, flame test, pH reading, and multiple tests for anions and cations. Once the compound was identified as NaCl, using the aforementioned tests, the tests were redone on the known compound NaCl and the same results to the tests were recorded for the UWC as NaCl. By combining HCl and NaOH, the compound was then synthesized, tested