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HomeSmall Molecules Analysis & Quality Control (QC)Gabapentin Assay and Related Substances Following Ph. Eur. Monograph Using Purospher® STAR RP-18e HPLC Column

Gabapentin Assay and Related Substances Following Ph. Eur. Monograph Using Purospher® STAR RP-18e HPLC Column

Ajay Kaparwan, Dr.

Mumbai Application Lab, India

Chemical structure of Gabapentin

Gabapentin

Introduction

Gabapentin is an anticonvulsant medication primarily used to treat partial seizures and neuropathic pain. It is a first-line medication for the treatment of neuropathic pain caused by diabetic neuropathy, post-therapeutic neuralgia, and central neuropathic pain.1 It is moderately effective - about 30-40% of those given gabapentin for diabetic neuropathy or post-therapeutic neuralgia have a meaningful benefit. Gabapentin acts by decreasing the activity of a subset of calcium channels.2

We demonstrate the assay and related substances determination of gabapentin following the Ph. Eur monograph using the Purospher® STAR RP-18 endcapped column, 250 x 4.6 mm, 5 μm.3

Gabapentin Assay and System Suitability Test

Blank chromatogram

Figure 1.Blank chromatogram.

Chromatogram of System suitability solution

Figure 2.Reference solution C for System suitability.

Chromatographic Data - System Suitability Solution

Chromatogram of Gabapentin test solution (14mg/mL)

Figure 3.Chromatogram of Gabapentin test solution (14mg/mL).

Chromatographic Data - Test Solution 14 mg/mL

Gabapentin Assay - Calibration

Calibration curve obtained for Gabapentin in its assay

Figure 4.Calibration function Gabapentin.

Table 1.Calibration data- Gabapentin

Assay of Gabapentin Related Substances A, B, and E and System Suitability Test

Chromatogram of Reference Solution A (14 mg/mL)

Figure 5.Reference solution A (14 mg/mL Gabapentin).

Chromatographic Data – Reference solution A, 14 µg/mL

Run time for impurity testing to be 4x retention time of Gabapentin = 20.06 min.

Chromatogram of Reference Solution B (Gabapentin Impurity A and B)

Figure 6.Reference solution B - Gabapentin impurity A and B.

Chromatographic Data – Reference Solution B

Table 2.Calibration Data- Gabapentin Related Substance A, B and E

Assay of Gabapentin Related Substance D

Chromatogram of Reference Solution OF Gabapentin Related Substance D

Figure 7.Reference Solution Gabapentin Related Substance D.

Test Solution: 14 mg/mL with Impurity D: 7 µg/mL

Figure 8.Test Solution 14 mg/mL substance showing 7.0 µg/mL Impurity D.

Chromatographic Data (Test Solution: 14 mg/ mL substance showing 7.0 µg/ mL Impurity D)

Table 3.Calibration Data- Gabapentin Related Substance D

Repeatability data and EP Criteria Gabapentin, Ph. Eur. Monograph

System Suitability

Table 4.System Suitability - Data of Gabapentin Reference Solution A (14 mg/mL) using Purospher® STAR RP-18e
Table 5.System Suitability - Data of Gabapentin Reference Solution C (14 mg/mL) using Purospher® STAR RP-18e
Table 6.System Suitability - Data of Gabapentin Reference Solution D (7 µg/mL) using Purospher® STAR RP-18e

Recovery of Gabapentin Related Substances A, B, D and E Spiked in Test solution (14 mg/mL), using Purospher® STAR RP-18e

Table 7.Recovery of Gabapentin Related Impurity A
Table 8.% Recovery of Gabapentin Related Impurity B
Table 9.% Recovery of Gabapentin Related Impurity D
Table 10.Recovery of Gabapentin Related Impurity E

Repeatability of Gabapentin Related Substances at LOQ levels using Purospher® STAR RP-18e

Table 11.Repeatability of Gabapentin Related Impurities at LOQ

Conclusion

The assay and related substances determination of gabapentin in pharmaceutical preparations with the Ph. Eur. monograph3 is demonstrated with the Purospher® Star RP-18 endcapped column, 250 X 4.6 mm, 5 μm.

The assay method shown, provided for gabapentin a Limit of Detection (LOD) of 0.55 µg/mL, and a Limit of Quantification (LOQ) of 1.68 µg/mL with linearity to a concentration of up to 21.0 µg/mL. The RSD on the repeatability of the gabapentin assay was <2%.

For the related substances A, B, D, and E of gabapentin, the Limit of Detection (LOD) ranged from 0.52 to 2.0 µg/mL and the Limit of Quantification (LOQ) was 1.58 to 6.06 µg/mL. Percentage recoveries ranged from 96.5 to 109.9%.

See more information on quality control testing at SigmaAldrich.com/PharmaQC

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References

1.
Attal N, Cruccu G, Baron R, Haanpää M, Hansson P, Jensen TS, Nurmikko T. 2010. EFNS guidelines on the pharmacological treatment of neuropathic pain: 2010 revision. Euro J of Neurology. 17(9):1113. https://doi.org/10.1111/j.1468-1331.2010.02999.x
2.
Wiffen PJ, Derry S, Bell RF, Rice AS, Tölle TR, Phillips T, Moore RA. Gabapentin for chronic neuropathic pain in adults. 2020(2): https://doi.org/10.1002/14651858.cd007938.pub4
3.
Ph. Eur. 11, 2173E. [Internet]. Available from: https://www.edqm.eu/en/european-pharmacopoeia-ph.-eur.-11th-edition
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