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Introduction: Biological reactions are catalyzed by enzymes. Many enzymes show a highly selective bePhysical Chemistry — Thermodynamics Chemistry Question

Enzymatic hydrolysis of N-acetyl alanine as an example of an environmentally benign process

Introduction:
Biological reactions are catalyzed by enzymes. Many enzymes show a highly selective behaviour and often are able to selectively catalyze reactions with one enantiomer of a racemate. In modern chemistry enzymes are used for many processes in vitro, especially for the synthesis of enantiomerically pure products. In this experiment the hydrolysis of N-acyl-alanine with the enzyme acylase I is investigated.

The process of the reaction can be monitored by following the formation of alanine using the reaction with ninhydrin, as shown below.

[VISUAL]

List of chemicals needed:
- rac. N-acetyl-alanine, 265 mg
- acylase I, 10 mg
- lithium hydroxide, 84 mg
- ninhydrine solution (Sigma N 1632), 2 cm3
- dimethyl sulfoxide, ca. 70 cm3
- lithium acetate buffer, pH 5.2.

Procedure:
Racemic N-acetyl-alanine (262 mg, 2.0 mmol) is dissolved in water (10 cm3). A solution of lithium hydroxide (84 mg, 2.0 mmol) in water (4 cm3) is then gradually added with gentle stirring. The pH is monitored with pH-paper until pH = 7 is reached. A solution of acylase I (10 mg) in water is added with vigorous stirring for 2 minutes. (The above enzyme solution is prepared by adding the enzyme to 5 cm3 of water and filtration using a small glass filter covered with diatomaceous earth.) Subsequently, water is added to reach the total volume of exactly 20.0 cm3. The reaction mixture is kept at a temperature of 37 °C in a water bath for 60 minutes. Then an accurate volume of 0.25 cm3 (use a syringe or a fine measuring pipette) is transferred into a test tube and ninhydrin (Sigma N 1632), (1.25 cm3) is added. This mixture is heated in boiling water during 20 minutes whereby a deep purple color is developed. After cooling, this mixture is accurately added to buffer solution consisting of 4 M lithium acetate aqueous buffer (pH = 5.2) and dimethyl sulfoxide in the ratio 1 : 3 in a volumetric flask of 250 cm3. Adjust the volume to 250 cm3. Then measure the absorbance of the solution at λ = 592 nm using a spectrophotometer. Use as a reference ninhydrin in the same lithium acetate buffer in dimethyl sulfoxide. ε (purple complex) = 13350 dm3 mol-1 cm-1.

Record the following data:
1. The initial concentration of racemic N.
2. The absorbance at λ = 592 nm.
3. Calculate the amount of substance (mmol) of alanine formed in the enzymatic reaction. Use the Lambert-Beer’s law.
4. Calculate the percentage of conversion.

Special note:
If time permits you may decide to stop the reaction after 10, 25, 40 and 60 minutes and determine the concentration of alanine in each case. Then construct a graph of the concentration of alanine vs. time and estimate the optimal reaction time.

29.1.

Will the alanine formed be optically active? (Yes or no.)

Model Answer

Yes.

29.2.

Will the N-acetyl-alanine that remains, be optically inactive, optically enriched or optically pure when the conversion is smaller than 50 %?

Model Answer

Optically enriched.

29.3.

Idem when the conversion is 50 % exactly?

Model Answer

Optically pure.

29.4.

Is the conversion larger than 50 % possible? (Yes or no.)

Model Answer

When the enzyme is highly selective: no.
When the enzyme is not highly selective: yes. In this case the preferred enantiomer will be hydrolyzed very fast and the other enantiomer will be converted more slowly.

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