Determination of mannitol content with Ultisil HILIC-Amide

1 comment

Test Report

Sample Information

Sample Name

Mannitol

Project Number

20230908-854-01

Sample Batch No.

/

Sample Characteristics

White powder

Sample Receipt Date

09/12/2023

Testing Period

09/18/2023 ~ 09/20/2023

Standard Sample Information

Name

Specification

Quantity

Mannitol

/

1

Requirement

Develop a method using an amino column with an ELSD detector so that the mannitol peak should not be affected by interference from other substances.

Reference Method

/

Reagent Information

Name

Grade

Brand

Acetonitrile

Chromatography

Welch

Instrument

Manufacturer

Type

Agilent

1260 (ELSD)

1. Experimental Process

1.1 Chromatographic Condition

Column

Ultisil® HILIC-Amide (4.6×250mm, 5μm)

Mobile Phase

Acetontitrile : water = 75:25

Flow Rate

1.0 mL/min

Injection Volume

10 μL

Column Temperature

30 °C

Detector

ELSD

Detector Temperature

80 °C

Carrier gas flow rate

1.8 L/min

Precautions

/

1.2 Solution Preparation

1.2.1 Preparation of mobile phase:

Acetonitrile: Use an appropriate amount of chromatography-grade acetonitrile and degas with ultrasonication.

Water: Use an appropriate amount of ultrapure water and degas with ultrasonication.

1.2.2 Preparation of mannitol standard solution:

Weigh an appropriate amount of mannitol raw material provided by the client, dissolve in water to prepare a solution with a concentration of approximately 0.3 mg/mL, and mix well.

1.2.3 Preparation of sample solutions:

Weigh an appropriate amount of the sample provided by the customer, dissolve in water to prepare a solution with a concentration of approximately 5 mg/mL, mix well, filter, and use the filtrate.

2. Chromatogram and Data: 

2.1 Chromatogram of blank solvent:

2.2 Chromatogram of standard solution:

 

Retention time (min) 

K

Area (mV*s)

Height (mV)

Symmetry Factor

Width (min)

Plates (USP)

Resolution (USP)

Selectivity

11.355

-

2691.67212

216.02324

1.11

0.1881

20184

-

--

2.3 Chromatogram of sample solution 1 (for method development):

Retention time (min) 

K

Area (mV*s)

Height (mV)

Symmetry Factor

Width (min)

Plates (USP)

Resolution (USP)

Selectivity

11.162

-

6483.72754

440.26373

1.03

0.2277

13311

-

--

2.4 Chromatogram of sample solution 2 (for testing):

Retention time (min) 

K

Area (mV*s)

Height (mV)

Symmetry Factor

Width (min)

Plates (USP)

Resolution (USP)

Selectivity

11.122

-

5244.35352

356.00610

1.14

0.2275

13241

-

--

3. Conclusion

Using the Welch Ultisil® HILIC-Amide (4.6×250mm, 5μm) under these chromatographic conditions, the mannitol peak exhibits good shape and retention without interference from other substances, meeting the client’s detection requirements.

1 comment

  • Need to analysis of Dapagliflozin with mannitol on same column and detector. plz suggest

    - Abhishek Jani

Post a comment

Please note, comments must be approved before they are published

Search Applications

Loading...