Aela Agela Technologies

Advance search
Quick Order
See your previous items:
You have 0 product(s) in cart

Preparation of Aclidinium Bromide

Application Introduction

Aclidinium bromide is a long-acting inhalant anticholinergic agent.

Favorite

Introduction

Aclidinium bromide is a long-acting inhalant anticholinergic agent. It can relax the muscle of lung tracheae and has been approved by FDA to be used for the long-term maintenance therapy of bronchospasm related to chronic obstructive pulmonary disease (COPD) in 2012. The peak tailing phenomenon often occurs if the sampling amount is increased during aclidinium bromide preparation. Therefore a packing which can solve peak tailing is needed.

Table 1 Aclidinium Bromide Sample Information

Sample   name

English   name

Structural   formula

Molecular   formula

Molecular   weight

CAS No.

Aclidinium bromide

Aclidinium bromide


C13H10BrN

564.56

320345-99-1

Experimental

Instrument, reagents and materials

FLEXATM purification system;

Deionized water; chromatographic solvents: acetonitrile and TFA;

High-performance liquid chromatographic columns: HLP (5 μm, 100 Å, 21.2 × 250 mm)

Venusil® ASB C18 (5 µm, 150 Å, 4.6 × 250 mm)

Sample dissolution

The sample is white powder. Dissolve 0.1 g of sample ultrasonically with 2 mL of solution mixed of acetonitrile and water (proporation: 1:1). Filter the sample with a 0.22 µm membrane, and then perform the sample loading.

Preparation conditions

Chromatographic columns: HLP (5 μm, 100 Å, 21.2 × 250 mm);

Mobile phases: A: TFA aqueous solution (concentration: 0.1 %), B: acetonitrile;

Wavelength: 222 nm

Flow rate: 18 mL/min

Sample size: 0.1 g

Gradient:

Table 2 Gradient Elution Conditions of Liquid Chromatography

Time/min

Flow rate/(mL/min)

A/%

B/%

0.0

18.0

90.0

10.0

30.0

18.0

10.0

90.0

Detection conditions

Chromatographic columns: ASB C18 (5 μm, 150 Å, 4.6 × 250 mm);

Mobile phases: A: TFA aqueous solution (concentration: 0.1 %), B: acetonitrile;

Wavelength: 222 nm

Flow rate: 1 mL/min

Sample size: 10 μL

Gradient:

Table 3 Gradient Elution Conditions of Liquid Chromatography

Time/min

Flow rate/(mL/min)

A/%

B/%

0.0

1.0

90.0

10.0

30.0

1.0

10.0

90.0

Results and Discussion

In this experiment, aclidinium bromide is prepared with HLP (5 μm, 100 Å, 21.2×250 mm) chromatographic columns. As shown in Table 2, Figure 1 and Figure 2, the sample preparation chromatogram shows a good peak shape and the sample is well separated from nearby impurities after the sample goes through the gradient elution in the mobile phases including TFA aqueous solution (concentration: 0.1 %) and acetonitrile. The freeze-drying equipment shall be used for the posttreatment because there is a lot of water in the receiving solution.

Besides, the chromatographic columns must be flushed with acetonitrile after every separation, otherwise the peak frontier will occur and it is unable to separate target object and impurity peaks. The expected peak shape will be shown after the chromatographic columns are flushed with acetonitrile.

Figure 1 Preparation Chromatogram

Figure 2 Distillate Detection Chromatogram

Conclusion

In this experiment, aclidinium bromide is prepared with HLP (5 μm, 100 Å, 21.2×250 mm) chromatographic columns. The detection purity of the product prepared through HLP high-pressure packing separation is higher than 99% and conforming to the requirement of customer.


  • Venusil ASB Series Columns (C1, C8, C18 and phenyl)

    The Venusil ASB series columns are specially designed for the separation of polar compounds under low (extremely stable at pH=0.8) to medium pH condition. The stationary phase is bonded with unique bulky silanes that sterically protect the siloxane bond. We offer a line of bonding chemistry of C1, C8, C18 or Phenyl groups presenting a broad selection of different polarity for various applications.

Material Name Material Type Date
Modify product number success!
Total Price:

Close

Email To Sombody

X
Email
Subject
Content

Login

X
Email address
Password
Register Forgotten your password?