Feasibility of Using Fluorescence Spectrophotometry to Develop a Sensitive Dye Immersion Method for Container Closure Integrity Testing of Prefilled Syringes

Xujin Lu; David K. Lloyd; Steven E. Klohr

doi:10.5731/pdajpst.2015.006015

References

1.↵
1. Adler M.
Challenges in the development of pre-filled syringes for biologics from a formulation scientist's point of view. Am. Pharm. Rev. 2012, 15 (1), 96–101.
OpenUrl
2.↵
1. Kiang P.
Recent developments in prefilled syringes. Am. Pharm. Rev. 2012, 15 (1), 104–107.
OpenUrl
3.↵
U. S. Food and Drug Administration (FDA). Guidance for Industry—Submission of Documentation for Sterilization Process Validation in Applications for Human and Veterinary Drug Products; FDA: Silver Spring, MD, 1994.
4.↵
European Commission. EU Guidelines to Good Manufacturing Practice Medicinal Products for Human and Veterinary Use. Annex 1, Manufacture of Sterile Medicinal Products; European Commission: Brussels, Belgium, 2008.
5.↵
FDA. Guidance for Industry—Container and Closure System Integrity Testing in Lieu of Sterility Testing as a Component of the Stability Protocol for Sterile Products; FDA: Silver Spring, MD, 2008.
6.↵
USP. General Chapter <1207> Sterile Product Packaging—Integrity Evaluation; United States Pharmacopeia; United States Pharmacopeial Convention: Rockville, MD, 2014; Vol. 37.
7.↵
1. Carroll M. C.,
2. Danny V. F.,
3. Guazzo D. M.,
4. Kaiser M. W.,
5. Kirsch L. E.,
6. Ludwig J. D.,
7. Masover G. K.,
8. May J. L.,
9. Moldenhauer J. E.,
10. Olsen J. I.,
11. Polsen T. M.,
12. Wright G.E.
Pharmaceutical Package Integrity; PDA Technical Report #27; Parenteral Drug Association: Bethesda, MD, 1998.
8.↵
1. Li L.
Container closure integrity testing method development and validation for prefilled syringes. Am. Pharm. Rev. 2013, 16 (1), 48–52.
OpenUrl
9.↵
1. Simonetti A.,
2. Amari F.
Non-destructive vacuum decay method for pre-filled syringe closure integrity testing compared with dye ingress testing and high-voltage leak detection. PDA J. Pharm. Sci. and Technol. 2015, 69 (1), 108–122.
OpenUrl
10.↵
1. Morton D. K.,
2. Lordi N. G.,
3. Ambrosio T. J.
Quantitative and mechanistic measurements of parenteral vial container/closure integrity, leakage quantitation. J. Parenter. Sci. Technol. 1989, 43 (2), 88–97.
OpenUrl PubMed
11.↵
1. Wolf H.,
2. Stauffer T.,
3. Chen S.-C. Y.,
4. Lee Y.,
5. Foster R.,
6. Ludzinski M.,
7. Kamat M.,
8. Godorov P.,
9. Guazzo D. M.
Vacuum decay container/closure integrity testing technology. Part 1. ASTM F2338–09 precision and bias studies. PDA J. Pharm. Sci. Technol. 2009, 63 (5), 472–488.
OpenUrl Abstract/FREE Full Text
12.↵
1. Wolf H.,
2. Stauffer T.,
3. Chen S.-C. Y.,
4. Lee Y.,
5. Foster R.,
6. Ludzinski M.,
7. Kamat M.,
8. Mulhall B.,
9. Guazzo D. M.
Vacuum decay container/closure integrity testing technology. Part 2. Comparison to dye ingress tests. PDA J. Pharm. Sci. Technol. 2009, 63 (5), 489–498.
OpenUrl Abstract/FREE Full Text
13.↵
1. Patel J.,
2. Mulhall B.,
3. Wolf H.,
4. Klohr S.,
5. Guazzo D. M.
Vacuum decay container closure integrity leak test method development and validation for a lyophilized product-package system. PDA J. Pharm. Sci. Technol. 2011, 65 (5), 486–505.
OpenUrl Abstract/FREE Full Text
14.↵
1. Kirsch L. E.,
2. Nguyen L.,
3. Moeckly C. S.
Pharmaceutical container/closure integrity I: Mass spectrometry–based helium leak rate detection for rubber-stoppered glass vials. PDA J. Pharm. Sci. Technol. 1997, 51 (5), 187–194.
OpenUrl Abstract/FREE Full Text
15.↵
1. Sudo H.,
2. O'driscoll M.,
3. Nishiwaki K.,
4. Kawamoto Y.,
5. Gammell P.,
6. Schramm G.,
7. Wertli T.,
8. Prinz H.,
9. Mori A.,
10. Sako K.
Development of a nondestructive leak testing method utilizing the head space analyzer for ampoule products containing ethanol-based solutions. PDA J. Pharm. Sci. Technol. 2012, 66 (5), 434–444.
OpenUrl Abstract/FREE Full Text
16.↵
1. Zuleger B.,
2. Werner U.,
3. Kort A.,
4. Glowienka R.,
5. Wehnes E.,
6. Duncan D.
Container/closure integrity testing and the identification of a suitable vial/stopper combination for low-temperature storage at −80 °C. PDA J. Pharm. Sci. Technol. 2012, 66 (5), 453–465.
OpenUrl Abstract/FREE Full Text
17.↵
1. Yoon S.-Y.,
2. Sagi H.,
3. Goldhammer C.,
4. Li L.
Mass Extraction Container Closure Integrity Physical Testing Method Development for Parenteral Container Closure Systems. PDA J. Pharm. Sci. Technol. 2012, 66 (5), 403–419.
OpenUrl Abstract/FREE Full Text
18.↵
1. Jacobus R. H.,
2. Torralba P.,
3. Moldenhauer J.,
4. Scheidt W. C.,
5. Runkle J. A.
Development and validation of a spectrophotometric dye immersion method used to measure container-closure integrity of an oil-based product. PDA J. Pharm. Sci. Technol. 1998, 52 (3), 110–112.
OpenUrl Abstract/FREE Full Text
19.↵
1. Burrell L. S.,
2. Carver M. W.,
3. DeMuth G. E.,
4. Lambert W. J.
Development of a dye ingress method to assess container–closure integrity: correlation to microbial ingress. PDA J. Pharm. Sci. Technol. 2000, 54 (6), 449–455.
OpenUrl Abstract/FREE Full Text
20.↵
1. Patel J.,
2. Tattersall P.,
3. Lloyd D.,
4. Gandhi H.,
5. Klohr S.
Development of a General Method for Container Closure Integrity Testing of Syringes. Poster #20, PDA Annual Conference, Phoenix, AZ, April 2012.
21.↵
1. Damgaard R.,
2. Rasmussen M.,
3. Buus P.,
4. Mulhall B.,
5. Guazzo D. M.
High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 1. Method development and validation. PDA J. Pharm. Sci. Technol. 2013, 67 (6), 634–651.
OpenUrl Abstract/FREE Full Text
22.↵
1. Rasmussen M.,
2. Damgaard R.,
3. Buus P.,
4. Mulhall B.,
5. Guazzo D. M.
High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 2. Method performance as a function of heat seal defects, product–package refrigeration, and package plastic laminate lot. PDA J. Pharm. Sci. Technol. 2013, 67 (6), 652–663.
OpenUrl Abstract/FREE Full Text
23.↵
1. Rasmussen M.,
2. Damgaard R.,
3. Buus P.,
4. Guazzo D. M.
High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 3. Chemical stability and visual appearance of a protein-based aqueous solution for injection as a function of HVLD exposure. PDA J. Pharm. Sci. Technol. 2013, 67 (6), 664–669.
OpenUrl Abstract/FREE Full Text
24.↵
USP. General Chapter <381> Elastomeric Closures for Injections; USP 32, 2009.
25.↵
EP. 3.2.9. Rubber Closures for Containers for Aqueous Parenteral Preparations, for Powders and for Freeze-Dried Powders; European Pharmacopeia 5.0, 2005.
26.↵
1. Akers M. J.
1. Guazzo D. M.
Sterile Product–Package Integrity Testing. In Sterile Drug Products, Formulation, Packaging, Manufacturing and Quality, Akers M. J., Ed.; Informa Healthcare: New York, 2010.
27.↵
1. Cenens J.,
2. Schoonheydt R. A.
Visible spectroscopy of methylene blue on hectorite, laponite, laponite B, and barasym in aqueous suspension. Clay and Clay Minerals 1988, 36 (3), 214–224.
OpenUrl Abstract
28.↵
1. Fujimoto B. S.,
2. Clendenning J. B.,
3. Delrow J. J.,
4. Heath P. J.,
5. Schurr M.
Fluorescence and photobleaching studies of methylene blue binding to DNA. J. Phys. Chem. 1994, 98 (26), 6633–6643.
OpenUrl CrossRef
29.
1. Kelly J. M.,
2. van der Putten W. J. M.,
3. Mcconnell D. J.
Laser flash spectroscopy of methylene blue with nucleic acids. Photochem. Photobiol. 2008, 45 (2), 167–175.
OpenUrl
30.↵
1. Du H.,
2. Fuh R. A.,
3. Li J.,
4. Corkan L. A.,
5. Lindsey J. S.
PhotochemCAD: a computer-aided design and research tool in photochemistry. Photochem. Photobiol. 1998, 68 (2), 141–142.
OpenUrl CrossRef Web of Science
31.↵
1. Kubin R. F.,
2. Fletcher A. N.
Fluorescence quantum yields of some Rhodamine dyes. J. Luminescence 1982, 27, 455–462.
OpenUrl CrossRef

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Keywords

[1] 1.↵
Adler M.
Challenges in the development of pre-filled syringes for biologics from a formulation scientist's point of view. Am. Pharm. Rev. 2012, 15 (1), 96–101.
OpenUrl

[2] Adler M.

[3] 2.↵
Kiang P.
Recent developments in prefilled syringes. Am. Pharm. Rev. 2012, 15 (1), 104–107.
OpenUrl

[4] Kiang P.

[5] 3.↵
U. S. Food and Drug Administration (FDA). Guidance for Industry—Submission of Documentation for Sterilization Process Validation in Applications for Human and Veterinary Drug Products; FDA: Silver Spring, MD, 1994.

[6] 4.↵
European Commission. EU Guidelines to Good Manufacturing Practice Medicinal Products for Human and Veterinary Use. Annex 1, Manufacture of Sterile Medicinal Products; European Commission: Brussels, Belgium, 2008.

[7] 5.↵
FDA. Guidance for Industry—Container and Closure System Integrity Testing in Lieu of Sterility Testing as a Component of the Stability Protocol for Sterile Products; FDA: Silver Spring, MD, 2008.

[8] 6.↵
USP. General Chapter <1207> Sterile Product Packaging—Integrity Evaluation; United States Pharmacopeia; United States Pharmacopeial Convention: Rockville, MD, 2014; Vol. 37.

[9] 7.↵
Carroll M. C.,
Danny V. F.,
Guazzo D. M.,
Kaiser M. W.,
Kirsch L. E.,
Ludwig J. D.,
Masover G. K.,
May J. L.,
Moldenhauer J. E.,
Olsen J. I.,
Polsen T. M.,
Wright G.E.
Pharmaceutical Package Integrity; PDA Technical Report #27; Parenteral Drug Association: Bethesda, MD, 1998.

[10] Carroll M. C.,

[11] Danny V. F.,

[12] Guazzo D. M.,

[13] Kaiser M. W.,

[14] Kirsch L. E.,

[15] Ludwig J. D.,

[16] Masover G. K.,

[17] May J. L.,

[18] Moldenhauer J. E.,

[19] Olsen J. I.,

[20] Polsen T. M.,

[21] Wright G.E.

[22] 8.↵
Li L.
Container closure integrity testing method development and validation for prefilled syringes. Am. Pharm. Rev. 2013, 16 (1), 48–52.
OpenUrl

[23] Li L.

[24] 9.↵
Simonetti A.,
Amari F.
Non-destructive vacuum decay method for pre-filled syringe closure integrity testing compared with dye ingress testing and high-voltage leak detection. PDA J. Pharm. Sci. and Technol. 2015, 69 (1), 108–122.
OpenUrl

[25] Simonetti A.,

[26] Amari F.

[27] 10.↵
Morton D. K.,
Lordi N. G.,
Ambrosio T. J.
Quantitative and mechanistic measurements of parenteral vial container/closure integrity, leakage quantitation. J. Parenter. Sci. Technol. 1989, 43 (2), 88–97.
OpenUrl PubMed

[28] Morton D. K.,

[29] Lordi N. G.,

[30] Ambrosio T. J.

[31] 11.↵
Wolf H.,
Stauffer T.,
Chen S.-C. Y.,
Lee Y.,
Foster R.,
Ludzinski M.,
Kamat M.,
Godorov P.,
Guazzo D. M.
Vacuum decay container/closure integrity testing technology. Part 1. ASTM F2338–09 precision and bias studies. PDA J. Pharm. Sci. Technol. 2009, 63 (5), 472–488.
OpenUrl Abstract/FREE Full Text

[32] Wolf H.,

[33] Stauffer T.,

[34] Chen S.-C. Y.,

[35] Lee Y.,

[36] Foster R.,

[37] Ludzinski M.,

[38] Kamat M.,

[39] Godorov P.,

[40] Guazzo D. M.

[41] 12.↵
Wolf H.,
Stauffer T.,
Chen S.-C. Y.,
Lee Y.,
Foster R.,
Ludzinski M.,
Kamat M.,
Mulhall B.,
Guazzo D. M.
Vacuum decay container/closure integrity testing technology. Part 2. Comparison to dye ingress tests. PDA J. Pharm. Sci. Technol. 2009, 63 (5), 489–498.
OpenUrl Abstract/FREE Full Text

[42] Wolf H.,

[43] Stauffer T.,

[44] Chen S.-C. Y.,

[45] Lee Y.,

[46] Foster R.,

[47] Ludzinski M.,

[48] Kamat M.,

[49] Mulhall B.,

[50] Guazzo D. M.

[51] 13.↵
Patel J.,
Mulhall B.,
Wolf H.,
Klohr S.,
Guazzo D. M.
Vacuum decay container closure integrity leak test method development and validation for a lyophilized product-package system. PDA J. Pharm. Sci. Technol. 2011, 65 (5), 486–505.
OpenUrl Abstract/FREE Full Text

[52] Patel J.,

[53] Mulhall B.,

[54] Wolf H.,

[55] Klohr S.,

[56] Guazzo D. M.

[57] 14.↵
Kirsch L. E.,
Nguyen L.,
Moeckly C. S.
Pharmaceutical container/closure integrity I: Mass spectrometry–based helium leak rate detection for rubber-stoppered glass vials. PDA J. Pharm. Sci. Technol. 1997, 51 (5), 187–194.
OpenUrl Abstract/FREE Full Text

[58] Kirsch L. E.,

[59] Nguyen L.,

[60] Moeckly C. S.

[61] 15.↵
Sudo H.,
O'driscoll M.,
Nishiwaki K.,
Kawamoto Y.,
Gammell P.,
Schramm G.,
Wertli T.,
Prinz H.,
Mori A.,
Sako K.
Development of a nondestructive leak testing method utilizing the head space analyzer for ampoule products containing ethanol-based solutions. PDA J. Pharm. Sci. Technol. 2012, 66 (5), 434–444.
OpenUrl Abstract/FREE Full Text

[62] Sudo H.,

[63] O'driscoll M.,

[64] Nishiwaki K.,

[65] Kawamoto Y.,

[66] Gammell P.,

[67] Schramm G.,

[68] Wertli T.,

[69] Prinz H.,

[70] Mori A.,

[71] Sako K.

[72] 16.↵
Zuleger B.,
Werner U.,
Kort A.,
Glowienka R.,
Wehnes E.,
Duncan D.
Container/closure integrity testing and the identification of a suitable vial/stopper combination for low-temperature storage at −80 °C. PDA J. Pharm. Sci. Technol. 2012, 66 (5), 453–465.
OpenUrl Abstract/FREE Full Text

[73] Zuleger B.,

[74] Werner U.,

[75] Kort A.,

[76] Glowienka R.,

[77] Wehnes E.,

[78] Duncan D.

[79] 17.↵
Yoon S.-Y.,
Sagi H.,
Goldhammer C.,
Li L.
Mass Extraction Container Closure Integrity Physical Testing Method Development for Parenteral Container Closure Systems. PDA J. Pharm. Sci. Technol. 2012, 66 (5), 403–419.
OpenUrl Abstract/FREE Full Text

[80] Yoon S.-Y.,

[81] Sagi H.,

[82] Goldhammer C.,

[83] Li L.

[84] 18.↵
Jacobus R. H.,
Torralba P.,
Moldenhauer J.,
Scheidt W. C.,
Runkle J. A.
Development and validation of a spectrophotometric dye immersion method used to measure container-closure integrity of an oil-based product. PDA J. Pharm. Sci. Technol. 1998, 52 (3), 110–112.
OpenUrl Abstract/FREE Full Text

[85] Jacobus R. H.,

[86] Torralba P.,

[87] Moldenhauer J.,

[88] Scheidt W. C.,

[89] Runkle J. A.

[90] 19.↵
Burrell L. S.,
Carver M. W.,
DeMuth G. E.,
Lambert W. J.
Development of a dye ingress method to assess container–closure integrity: correlation to microbial ingress. PDA J. Pharm. Sci. Technol. 2000, 54 (6), 449–455.
OpenUrl Abstract/FREE Full Text

[91] Burrell L. S.,

[92] Carver M. W.,

[93] DeMuth G. E.,

[94] Lambert W. J.

[95] 20.↵
Patel J.,
Tattersall P.,
Lloyd D.,
Gandhi H.,
Klohr S.
Development of a General Method for Container Closure Integrity Testing of Syringes. Poster #20, PDA Annual Conference, Phoenix, AZ, April 2012.

[96] Patel J.,

[97] Tattersall P.,

[98] Lloyd D.,

[99] Gandhi H.,

[100] Klohr S.

[101] 21.↵
Damgaard R.,
Rasmussen M.,
Buus P.,
Mulhall B.,
Guazzo D. M.
High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 1. Method development and validation. PDA J. Pharm. Sci. Technol. 2013, 67 (6), 634–651.
OpenUrl Abstract/FREE Full Text

[102] Damgaard R.,

[103] Rasmussen M.,

[104] Buus P.,

[105] Mulhall B.,

[106] Guazzo D. M.

[107] 22.↵
Rasmussen M.,
Damgaard R.,
Buus P.,
Mulhall B.,
Guazzo D. M.
High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 2. Method performance as a function of heat seal defects, product–package refrigeration, and package plastic laminate lot. PDA J. Pharm. Sci. Technol. 2013, 67 (6), 652–663.
OpenUrl Abstract/FREE Full Text

[108] Rasmussen M.,

[109] Damgaard R.,

[110] Buus P.,

[111] Mulhall B.,

[112] Guazzo D. M.

[113] 23.↵
Rasmussen M.,
Damgaard R.,
Buus P.,
Guazzo D. M.
High-voltage leak detection of a parenteral proteinaceous solution product packaged in form-fill-seal plastic laminate bags. Part 3. Chemical stability and visual appearance of a protein-based aqueous solution for injection as a function of HVLD exposure. PDA J. Pharm. Sci. Technol. 2013, 67 (6), 664–669.
OpenUrl Abstract/FREE Full Text

[114] Rasmussen M.,

[115] Damgaard R.,

[116] Buus P.,

[117] Guazzo D. M.

[118] 24.↵
USP. General Chapter <381> Elastomeric Closures for Injections; USP 32, 2009.

[119] 25.↵
EP. 3.2.9. Rubber Closures for Containers for Aqueous Parenteral Preparations, for Powders and for Freeze-Dried Powders; European Pharmacopeia 5.0, 2005.

[120] 26.↵
Akers M. J.
Guazzo D. M.
Sterile Product–Package Integrity Testing. In Sterile Drug Products, Formulation, Packaging, Manufacturing and Quality, Akers M. J., Ed.; Informa Healthcare: New York, 2010.

[121] Akers M. J.

[122] Guazzo D. M.

[123] 27.↵
Cenens J.,
Schoonheydt R. A.
Visible spectroscopy of methylene blue on hectorite, laponite, laponite B, and barasym in aqueous suspension. Clay and Clay Minerals 1988, 36 (3), 214–224.
OpenUrl Abstract

[124] Cenens J.,

[125] Schoonheydt R. A.

[126] 28.↵
Fujimoto B. S.,
Clendenning J. B.,
Delrow J. J.,
Heath P. J.,
Schurr M.
Fluorescence and photobleaching studies of methylene blue binding to DNA. J. Phys. Chem. 1994, 98 (26), 6633–6643.
OpenUrl CrossRef

[127] Fujimoto B. S.,

[128] Clendenning J. B.,

[129] Delrow J. J.,

[130] Heath P. J.,

[131] Schurr M.

[132] 29.
Kelly J. M.,
van der Putten W. J. M.,
Mcconnell D. J.
Laser flash spectroscopy of methylene blue with nucleic acids. Photochem. Photobiol. 2008, 45 (2), 167–175.
OpenUrl

[133] Kelly J. M.,

[134] van der Putten W. J. M.,

[135] Mcconnell D. J.

[136] 30.↵
Du H.,
Fuh R. A.,
Li J.,
Corkan L. A.,
Lindsey J. S.
PhotochemCAD: a computer-aided design and research tool in photochemistry. Photochem. Photobiol. 1998, 68 (2), 141–142.
OpenUrl CrossRef Web of Science

[137] Du H.,

[138] Fuh R. A.,

[139] Li J.,

[140] Corkan L. A.,

[141] Lindsey J. S.

[142] 31.↵
Kubin R. F.,
Fletcher A. N.
Fluorescence quantum yields of some Rhodamine dyes. J. Luminescence 1982, 27, 455–462.
OpenUrl CrossRef

[143] Kubin R. F.,

[144] Fletcher A. N.

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