Doxycycline Prolonged-release Capsules – BP 2019

These chromatograms are provided for information only as an aid to analysts and are intended as
guidance for the interpretation and application of BP monographs.

Typical chromatogram for solution (3) in the Related Substances test for Doxycycline Prolonged-release
Capsules as published in BP 2019.

12 12

10 10

8 8

6 6
mAU

mAU
4 1 4

2 2

0 0

4
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44
Minutes

Peak ID: 1: Impurity C; 2: Impurity A; 3: Impurity B; 4: Doxycycline; 5: Impurity F

Column : Waters, XTerra RP18 (250 mm x 4.6 mm, 5 μm)

Solution A : 11.16 % w/v solution of ethylenediaminetetracetic acid disodium salt dihydrate,
adjusted to pH 7.0 with concentrated ammonia (35 %)
Buffer : 6.79 % w/v tetrabutylammonium hydrogen sulfate solution adjusted to pH 7.0
with concentrated ammonia (35 %)
Mobile Phase : Acetonitrile: water: buffer: solution A (13: 17: 35: 35, v/v/v/v)
Diluent : 0.01 M hydrochloric acid
Flow Rate : 1 mL/min
Column Temp : 35°C
Injection Volume : 20 µL
Detection : UV, 280 nm
Typical chromatogram for solution (2) in the Assay test for Doxycycline Prolonged-release Capsules as
published in BP 2019.

35 35

30 30

25 25

20 20
mAU

mAU
15 15

10 10

5 5

0 0

1
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Minutes

Peak ID: 1: Doxycycline

Column : Waters, XTerra RP18 (250 mm x 4.6 mm, 5 μm)

Solution A : 11.16 % w/v solution of ethylenediaminetetracetic acid disodium salt dihydrate,
adjusted to pH 7.0 with concentrated ammonia (35 %)
Buffer : 6.79 % w/v tetrabutylammonium hydrogen sulfate solution adjusted to pH 7.0
with concentrated ammonia (35 %)
Mobile Phase : Acetonitrile: water: buffer: solution A (13: 17: 35: 35, v/v/v/v)
Diluent : 0.01 M hydrochloric acid.
Flow Rate : 1 mL/min
Column Temp : 35°C
Injection Volume : 20 µL
Detection : UV, 280 nm