comparison between disposable and conventional

1
Comparison between disposable and conventional chromatography in purification of r-h FSH M. Fahim 1 , F. Mueller 1 , J. Rohde 1 1 Rhein-Minapharm Biogenetics, R&D, Mina Street, 3rd Industrial Zone A2, 10th of Ramadan City, Egypt, The use of disposables in downstream processes is well established in terms of different filtration technologies, buffer preparation and storage of liquids and became increasingly popular over the last years. Disposable systems are generally known to have several significant advantages in comparison to conventional concepts such as risk reduction for cross contamination. Disposables also save costs, reduce buffer consumption [1], labor and capital space and minimize time of cleaning and cleaning validation of approximately 30% [2]. Recently, a number of new technologies for single use chromatography systems attracted many applicants to integrate them in downstream process strategies [3]. We explored disposable chromatography as a capture and/or intermediate step [Sartobind ® Q and Sartobind ® Phenyl] [4] in a defined purification process of r-h FSH. We herein compare the conventional chromatography pathway (P1) and alternative pathways which include one or two disposable chromatography steps (P2 and P3 ) in respect to their elution profile, yield and purity of the target protein. Results were found to be comparable with several advantages of the disposable membrane Introduction [email protected] adsorber , in addition to the above mentioned benefits; the disposable membrane adsorber solved a carryover problem monitored with the traditional chromatography in the capture step. Process flow chart r-h FSH in ultra filtered supernatant Path a 2 3 Capture step (IEC) Intermediate step (HIC Phenyl) Polishing step (HICOctyl) Pathway 1 Pathway 2 Pathway 3 Pathway 1 Pathway 2 Pathway 3 Pathway 1 Pathway 2 Pathway 3 Q Sartobind Sartobind Phenyl Phenyl Sartobind 1- RP-HPLC Results and discussion Pathway 1 Conventional columns (1) Q-Sepharose Y= 60% (2) Pathway 2 One disposable step (1) Sartobind Q Y= 72% (2) Pathway 3 Two disosable steps (1) Sartobind Q Y=73% (2) Sartobind Column QSepharose Sartobind Q Sartobind Q Phenyl HP Phenyl HP Sartobind Phenyl Octyl Octyl Octyl FSH loaded [mg] 6.25 8.63 8.63 3.13 4.24 1.96 1.04 1.3 0.99 FSH loaded per ml resin [mg/mL] 1.25 1.23 1.23 0.62 0.84 0.65 0.20 0.26 0.19 Eluted FSH [mg] 3.81 6.24 6.30 1.10 1.68 0.96 0.67 0.84 0.58 Yield [%] 60.96 72.30 73.00 35.14 39.62 48.97 64.42 64.61 58.58 Recovery [%] 84.32 88.99 92.46 78.91 100.00 81.63 91.34 100.00 88.88 Comments Comparable elution profiles with higher yield for the disposable column ( Sartobind Q) in Different elution steps with different profiles due to early elution in case of the disposable column (Sartobind Comparable profiles and yields Phenyl HP Y= 35% (3) Octyl Y= 64% Overall yield 13% Phenyl HP Y= 39% (3) Octyl Y= 64% Overall yield 18% Sartobind Phenyl Y= 48% (3) Octyl Y= 58% Overall yield 20% comparison to the conventional one (QSepharose) Phenyl) but with higher yield in comparison to the conventional one (Phenyl HP) 2- SDS-PAGE & Western blot KDa 116.3 97.4 66.3 55.4 Table1 presents overview of the RP-HPLC analysis results of the three different pathways (P1, P2 and P3). rh FSH before purification rh FSH after purification Intact purified FSH P1 P2 P3 St. KDa 116.3 97.4 66.3 55.4 P1 P2 P3 St. Lane Sample Name Lane Sample Name 1 Marker 2 Supernatant 3 Purified FSH (Pathway1) 150IU 4 Purified FSH (Pathway1) 75IU 5 Purified FSH (Pathway2) 150IU 6 Purified FSH (Pathway2) 75IU 7 Purified FSH (Pathway3) 150IU 8 Purified FSH (Pathway3) 75IU Figure 2 presents Silver stained SDS-PAGE and Western Blot of supernatant containing r-h FSH before and after purification by the three different pathways (P1, P2 and P3). Main fraction containing purified r-h FSH diluted to 150 and 75 IU in comparison to standard with the same concentration. Materials: Q-Sepharose FF column; CV= 5mL, Phenyl HP ® column; CV= 5mL, Sartobind ® Q membrane; CV= 7mL, Sartobind ® Phenyl membrane; CV= 3mL, Octyl FF ® column; CV= 5mL, ÄKTA explorer 100. Materials and Methods 36.5 31.5 21.5 14.4 Figure1 presents flow chart of the three different purification pathways (P1, P2 and P3); Y= Yield. 12 1 3 4 5 6 7 8 910 1 3 4 5 6 7 8 910 Degraded FSH 36.5 31.5 21.5 14.4 Remaining impurity Conclusions and outlook 9 Standard r-h FSH 150IU 10 Standard r-h FSH 75IU Disposable chromatography systems have several advantages in comparison to conventional columns. They minimize time of cleaning and cleaning validation and solve the carry over problem specially in the capture step. That encouraged us to apply it in different steps in the purification process of r-h FSH which is under development. Application of one disposable chromatography step (Sartobind Q) in the capture step of r-h FSH purification process was comparable to the conventional column (Q-sepharose) regarding the elution profiles and purity. An additional advantage i i th i ld b 10% f thi t d 5% f th ll i ld Methods: Ultra filtered CHO culture supernatant containing r-h FSH was purified as follows: [P1]: Application of conventional columns: Capturing (Q- Sepharose), intermediate purification (Phenyl HP) and polishing (Octyl FF) of r-h FSH. 1.25, 0.62 and 0.2 mg FSH were loaded per [ml] resin on the three different columns. [P2]: Application of one disposable chromatography capture step using Sartobind Q with subsequent continuation of purification by conventional columns (Phenyl HP and Octyl). 1.23, 0.84 and 0.26 mg FSH were loaded per [ml] resin. References: [1] Govind Rao et al. Non Invasive Sensors as Enablers of “Smart” Disposables. BioProcess International. 2009; vol.7, supplement1 [2] D'Aquino, Rita: Bioprocessing Systems Go Disposable. Chemical Engineering Progress May 2006. [3] Disposables Improve Downstream Process. Euro Bio Tech News.2008; vol.7,7-8 [4] Stefan Fischer. Sartobind Membrane Adsorbers. August 2009 (www.sartorius.com). was an increase in the yield by 10% for this step and 5% for the overall yield. Application of two disposable chromatography steps (Sarobind Q and Sarobind Phenyl) in the capture and intermediate step of the r-h FSH purification process showed a minimal decrease in final product purity but the overall yield increased by 7%. Further development for the Sartobind phenyl step is still needed to improve the final product purity and maintain the high yield. Future applications in different pipeline processes are currently under evaluation. [P3]: Involved the application of two disposable chromatography steps (capture and intermediate) using Sartobind Q and Sartobind Phenyl, followed by conventional polishing (Octyl FF).1.23, 0.65 and 0.19 mg FSH were loaded per ml resin. Flow rate: 5 mL/min. All fractions eluted were analyzed by RP-HPLC and silver stained SDS-PAGE as well as Western Blot.

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Comparison between disposable and conventional chromatography in purification

of r-h FSH M. Fahim1, F. Mueller1, J. Rohde1

1Rhein-Minapharm Biogenetics, R&D, Mina Street, 3rd Industrial Zone A2, 10th of Ramadan City, Egypt,

The use of disposables in downstream processes is well established in terms of different filtration technologies, buffer preparation and storage of liquids and became increasingly popular over the last years. Disposable systems are generally known to have several significant advantages in comparison to conventional concepts such as risk reduction for cross contamination. Disposables also save costs, reduce buffer consumption [1], labor and capital space and minimize time of cleaning and cleaning validation of approximately 30% [2]. Recently, a number of new technologies for single use chromatography systems attracted many applicants to integrate them in downstream process strategies [3]. We explored disposable chromatography as a capture and/or intermediate step [Sartobind® Q and Sartobind® Phenyl] [4] in a defined purification process of r-h FSH. We herein compare the conventional chromatography pathway (P1) and alternative pathways which include one or two disposable chromatography steps (P2 and P3 ) in respect to their elution profile, yield and purity of the target protein. Results were found to be comparable with several advantages of the disposable membrane

[email protected]

adsorber, in addition to the above mentioned benefits; the disposable membrane adsorber solved a carryover problem monitored with the traditional chromatography in the capture step.

Process flow chartr-h FSH in

ultra filteredsupernatant

Path a 2 3

Capture step (IEC)

Intermediate step (HIC ‐ Phenyl)

Polishing step(HIC‐ Octyl)

Pathway 

1Pathway 

2Pathway 

3Pathway

1Pathway 

2Pathway

3Pathway 

1Pathway 

2Pathway 

3Q Sartobind Sartobind Phenyl Phenyl Sartobind

1- RP-HPLCResults and discussion

Pathway 1Conventional

columns

(1) Q-Sepharose

Y= 60%

(2)

Pathway 2One

disposable step

(1) Sartobind Q

Y= 72%

(2)

Pathway 3Two

disosablesteps

(1) Sartobind Q

Y=73%

(2) Sartobind

ColumnQ‐

SepharoseSartobind

QSartobind

QPhenyl HP

Phenyl HP

Sartobind Phenyl

Octyl Octyl Octyl

FSH loaded [mg] 6.25 8.63 8.63 3.13 4.24 1.96 1.04 1.3 0.99

FSH loaded per ml resin [mg/mL]

1.25 1.23 1.23 0.62 0.84 0.65 0.20 0.26 0.19

Eluted FSH [mg] 3.81 6.24 6.30 1.10 1.68 0.96 0.67 0.84 0.58Yield [%] 60.96 72.30 73.00 35.14 39.62 48.97 64.42 64.61 58.58

Recovery [%] 84.32 88.99 92.46 78.91 100.00 81.63 91.34 100.00 88.88

Comments

Comparable elution profiles with higher yield for the disposable 

column ( Sartobind Q) in 

Different elution steps with different profiles due to early 

elution in case of the disposable column (Sartobind

Comparable profiles and yields

Phenyl HPY= 35%

(3) Octyl

Y= 64%

Overall yield13%

Phenyl HPY= 39%

(3) Octyl

Y= 64%

Overall yield18%

SartobindPhenylY= 48%

(3) Octyl

Y= 58%

Overall yield20%

( )comparison to the conventional 

one (Q‐Sepharose)

p (Phenyl)  but with higher yield 

in comparison to the conventional one (Phenyl HP)

2- SDS-PAGE & Western blot

KDa

116.397.466.3 55.4

Table1 presents overview of the RP-HPLC analysis results of the three different pathways (P1, P2 and P3).

r‐h FSH before purification r‐h FSH after purification

Intact purified FSH

P1      P2         P3     St.KDa

116.397.466.3 55.4

P1      P2         P3     St.

Lane Sample Name Lane Sample Name1 Marker 2 Supernatant3 Purified FSH (Pathway1) 150IU 4 Purified FSH (Pathway1) 75IU5 Purified FSH (Pathway2) 150IU 6 Purified FSH (Pathway2) 75IU7 Purified FSH (Pathway3) 150IU 8 Purified FSH (Pathway3) 75IU

Figure 2 presents Silver stained SDS-PAGE and Western Blot of supernatant containing r-h FSH before and after purification by the three different pathways (P1, P2 and P3). Main fraction containing purified r-h FSH diluted to 150 and 75 IU in comparison to

standard with the same concentration.Materials: Q-Sepharose FF column; CV= 5mL, Phenyl HP ® column; CV= 5mL, Sartobind® Q membrane; CV= 7mL, Sartobind ® Phenyl membrane; CV= 3mL, Octyl FF ® column; CV= 5mL, ÄKTA explorer 100.

Materials and Methods

36.5 31.5

21.5

14.4

Figure1 presents flow chart of the three different purification pathways (P1, P2 and P3); Y= Yield.

1 2 1    3     4    5   6    7    8  910 1       3     4    5   6   7   8   910

Degraded FSH

36.5 31.5

21.5

14.4Remaining impurity

Conclusions and outlook9 Standard r-h FSH 150IU 10 Standard r-h FSH 75IU

Disposable chromatography systems have several advantages in comparison to conventional columns. They minimize time of cleaning and cleaning validation and solve the carry over problem specially in the capture step. That encouraged us to apply it in different steps in the purification process of r-h FSH which is under development.

Application of one disposable chromatography step (Sartobind Q) in the capture step of r-h FSH purification process was comparable to the conventional column (Q-sepharose) regarding the elution profiles and purity. An additional advantage

i i th i ld b 10% f thi t d 5% f th ll i ld

Methods:Ultra filtered CHO culture supernatant containing r-h FSH was purified as follows:

[P1]: Application of conventional columns: Capturing (Q-Sepharose), intermediate purification (Phenyl HP) and polishing(Octyl FF) of r-h FSH. 1.25, 0.62 and 0.2 mg FSH were loaded per[ml] resin on the three different columns.

[P2]: Application of one disposable chromatography capture stepusing Sartobind Q with subsequent continuation of purification byconventional columns (Phenyl HP and Octyl). 1.23, 0.84 and 0.26mg FSH were loaded per [ml] resin.

References:[1] Govind Rao et al. Non Invasive Sensors as Enablers of “Smart” Disposables. BioProcess International. 2009; vol.7, supplement1[2] D'Aquino, Rita: Bioprocessing Systems Go Disposable. Chemical Engineering Progress May 2006.[3] Disposables Improve Downstream Process. Euro Bio Tech News.2008; vol.7,7-8[4] Stefan Fischer. Sartobind Membrane Adsorbers. August 2009 (www.sartorius.com).

was an increase in the yield by 10% for this step and 5% for the overall yield.

Application of two disposable chromatography steps (Sarobind Q and SarobindPhenyl) in the capture and intermediate step of the r-h FSH purification processshowed a minimal decrease in final product purity but the overall yield increasedby 7%. Further development for the Sartobind phenyl step is still needed toimprove the final product purity and maintain the high yield. Future applicationsin different pipeline processes are currently under evaluation.

g p [ ][P3]: Involved the application of two disposable chromatography

steps (capture and intermediate) using Sartobind Q and SartobindPhenyl, followed by conventional polishing (Octyl FF).1.23, 0.65 and0.19 mg FSH were loaded per ml resin.Flow rate: 5 mL/min. All fractions eluted were analyzed by RP-HPLCand silver stained SDS-PAGE as well as Western Blot.