Research progress in bacterial endotoxin test methods for insoluble raw materials, excipients and preparations

doi:10.19803/j.1672-8629.20230423

Abstract

Abstract: Objective To summarize the ideas behind test methods established for insoluble samples in the Chinese Pharmacopoeia and related literature in China over the past 10 years, and to provide reference for endotoxin detection of insoluble APIs, excipients and preparations. Methods The determination of endotoxin limits, inspection methods, dissolution methods, and strategies for excluding interferences in domestic literature on insoluble samples were analyzed by focusing on the selection of organic solvents. Results and conclusion The difficulty in establishing a method for the detection of bacterial endotoxin in insoluble samples lies in the search for suitable solvents and the elimination of interferences. Dissolution methods involve organic solvents, non-organic solvents and physical methods, while the elimination of interferences involves the adjustment of pH, the supplementation of divalent cations, and the use of antiproliferative fluids and dispersants. This study is expected to inspire ideas for subsequent research.

Key words: raw materials, excipients, preparations, bacterial endotoxin, TAL, insolubility, methodology, quality safety, elimination of interference

CLC Number:

R927.1

ZHANG Chenxue, PEI Yusheng, CAI Tong. Research progress in bacterial endotoxin test methods for insoluble raw materials, excipients and preparations[J]. Chinese Journal of Pharmacovigilance, 2024, 21(3): 273-279.

Add to citation manager EndNote|Ris|BibTeX

URL: https://www.zgywjj.com/EN/10.19803/j.1672-8629.20230423

https://www.zgywjj.com/EN/Y2024/V21/I3/273

References

[1] Chinese Pharmacopoeia Commission.Pharmacopoeia of the People's Republic of China Vol 4(中华人民共和国药典四部)[M]. Beijing: China Medical Science Press, 2020: 178-181, 474, 515-517.
[2] The United States Pharmacopeial Convention. U.S.Pharmacopeia [M]. Baltimore: United Book Press, 2020.
[3] Commission European Pharmacopoeia.European Pharmacopoeia[S]. European Directorate for the Quality of Medicines & HealthCare, 2022.
[4] LIU Q, LU YH.Study on the determination method of the bacterial endotoxins in fulvestrant[J]. Journal of Pharmaceutical Research(药学研究), 2014, 33(12): 696-698.
[5] YAN CQ, HUANG MM, WANG HP, et al.Establishment of bacterial endotoxin test for an insoluble drug substance[J]. China Pharmacist(中国药师), 2018, 21(2): 365-368.
[6] WU LL, LIU Y, LIU Q, et al.Study on the method of bacterial endotoxin test in bortezomib[J]. Journal of Pharmaceutical Research(药学研究), 2014, 25(13): 210-212.
[7] WANG D, ZHU SM, KUANG R.Bacterial endotoxins test for tacrolimus[C]. China Medicine Education Association(中国医药教育协会第三届三次理事大会暨学术年会论文专辑), 2013: 245-249.
[8] WANG H, WANG YY, XIE YH, et al.Investigation on bacterial endotoxin test method for levofloxacin hydrochloride[J]. Drug Standards of China(中国药品标准), 2021, 22(5): 478-482.
[9] LIU XF, WANG K, XU EM, et al.Investigation of methodological bacterial endotoxin test of ceftiofur hydrochloride[J]. Modern Journal of Animal Husbandry and Veterinary Medicine(现代畜牧兽医), 2022, 4: 17-20.
[10] XIA B, GUO F.Content determination of bacterial endotoxin in gatifloxacin by kinetic chromogenic analysis[J]. Chinese Journal of Drug Evaluation(中国药物评价), 2015, 32(5): 273-276.
[11] WEN YM, FAN JH, WU WQ, et al.Determination of bacterial endotoxin content in sirolimus API by adding surfactant[J]. Chinese Pharmaceutical Affairs(中国药事), 2022, 36(3): 301-305.
[12] ZHANG Y, QIU X, YIN YP.Establishment of bupivacaine bacterial endotoxin detection method[J]. Guangdong Chemical Industry(广东化工), 2020, 47(9): 188-190.
[13] ZHOU B, ZANG XH, GU J.Validation for bacterial endotoxin test method of propofol API[J]. Food and Drug(食品与药品), 2016, 18(5): 339-343.
[14] XU LM, WU G, DU WF, et al.Establishment of bacterial endotoxin test method for milrinone raw material[J]. Chin J Mod Appl Pharm(中国现代应用药学), 2014, 31(9): 1110-1114.
[15] WU LM, LI YJ, WEI X, et al.Quality specification study of bacterial endotoxin test in clevidipine butyrate[J]. Journal of Pharmaceutical Research(药学研究), 2013, 32(12): 702-704.
[16] XU LM, WU G, DU WF, et al.Bacterial endotoxin test for clevidipine butyrate[J]. Chin JMAP(中国现代应用药学), 2013, 30(9): 1004-1008.
[17] CHEN C, PEI YS, DU Y, et al.Bacterial endotoxin test methodology of vinpocetine active pharmaceutical ingredients[J]. China Pharmaceuticals(中国药业), 2021, 30(22): 78-81.
[18] ZHAO WQ, ZHAO YL, FU Q, et al.Detection of bacterial endotoxin in donepezil pamoate by dichloromethane extraction[J]. China Pharmaceuticals(中国药业), 2021, 30(3): 45-49.
[19] ZHANG P.Investigation on feasibility of bacterial endotoxin test for risperidone[J]. Strait Pharmaceutical Journal(海峡药学), 2021, 33(12): 69-71.
[20] LUO D.Methodological study on the bcaterial endotoxin test in elemene emulsion injection[D]. Shenyang: Shenyang Agricultural University(沈阳农业大学), 2022.
[21] CAO XF, HE HH, WU T, et al.Study on gelation clotmethod of bacterial endotoxin test in the burn ointment[J]. China Medcine and Pharmacy(中国医科药学), 2018, 8(19): 65-68.
[22] LIU Y, WANG Y, MENG CH, et al.Study on bacterial endotoxin test of octreotide acetate microspheres for injection[J]. Chinese Journal of New Drugs(中国新药杂志), 2021, 30(14): 1340-1344.
[23] PEI YS, LIU Y, CAI T, et al.Study on bacterial endotoxin detection method of three types of microsphere preparation[J]. Journal of Shenyang Pharmaceutical University(沈阳药科大学学报), 2022, 39(11): 1327-1332.
[24] PEI YS, CAI T, ZHANG GL, et al.Detection of bacterial endotoxin in paclitaxel liposome[J]. JournaL of Chinese PharmaceuticaL Sciences(中国药学杂志), 2018, 27(6): 436-441.
[25] SUN D.Methods for testing pyrogen and bacterial endotoxin in etoposideloaded lipid microsphere injection[J]. China Medicine and Pharmacy(中国医药科学), 2022, 12(3): 71-74,90.
[26] CHEN C, ZHAO XY, PEI YS.Study on bacterial endotoxin test of cholesterol[J]. Chin J Mod Appl Pharm(中国现代应用药学), 2023, 40(1): 82-85.
[27] ZHOU QL, GE HL, XU YQ.Study on bacterial endotoxin test method of egg yolk lecithin[J]. Chemical Industry Times(化工时刊), 2019, 33(9): 11-14.
[28] PEI YS, ZHAO XY, CHEN C, et al.Study on bacterial endotoxin detection of egg yolk lecithin of Chinese Pharmacopoeia 2020 Edition[J]. Chinese Pharmacological Bulletin(中国药理学通报), 2022, 38(8): 1227-1230.
[29] WAN LQ, GU SY, TANG LM.Quantitation of the bacterial endotoxin in oleic acid[J]. Chinese Journal of Pharmaceuticals(中国医药工业杂志), 2016, 47(5): 611-613.
[30] LIU XL, YUAN K, ZHAO D, et al.Establishment of the bacterial endotoxin test method of hydrogenated soybean lecithin through trichloromethane vibration extraction method[J]. Hebei Medical Journal(河北医药), 2021, 43(5): 780-783.
[31] PEI YS, CHEN C, CAI T, et al.Comparison and interpretation of guidelines for the application of bacterial endotoxin tests in Chinese and American Pharmacopoeia[J]. Chinese Journal of Pharmacovigilance(中国药物警戒), 2023, 20(3): 317-320, 330.
[32] PAUL H, DONNA CL, ROBERT AR, et al.The release and detection of endotoxin from liposomes[J]. Analytical Biochemistry, 1997, 250: 139-146.
[33] ZHU QF, ZHANG J, ZHU R, et al.Considerations on defining of bacterial endotoxin specifications for pharmaceutical excipients in Chinese Pharmacopeia[J]. Chin Pharm J(中国药学杂志), 2023, 58(7): 643-648.
[34] GONG W, WANG JD.Establishment of bacterial endotoxin test for clevidipine butyrate[J]. Strait Pharmaceutical Journal(海峡药学), 2015, 27(10): 41-43.
[35] DING SS, MA RQ, LIU H, et al.Establishment and comparison of pyrogen test and bacterial endotoxin test for lentinan API[J]. Chinese Journal of New Drugs(中国新药杂志), 2019, 28(15): 1896-1901.
[36] HAO M, JIAO J, LIU JP.Establishment of bacterial endotoxin test for doxercalciferol[J]. Drug Standards of China(中国药品标准), 2020, 21(6): 526-530.
[37] CHEN X, HE LM, LIU R.Progress on detection of bacterial endotoxin[J]. Chinese Journal of Analysis Laboratory(分析实验室), 2023, 9: 1242-1250.
[38] CHEN WN, CHEN JL, ZENG HZ, et al.Bacterial endotoxin test of dantrolene sodium[J]. China Medcine and Pharmacy(中国医药科学), 2017, 7(3): 53-56.
[39] LIN JH, CHEN XJ, DING YL.Study on the bacterial endotoxin test in the raw material of bromhexine hydrochloride for injection[J]. Shanghai Medical & Pharmaceutical Journal(上海医药), 2020, 41(7): 75-77.
[40] WAGN X, ZHANG GW, ZHANG JX.Establishment of thioctic acid bacterial endotoxin test[J]. Henan Medical Research(河南医学研究), 2020, 29(8): 1369-1372.
[41] FENG M, YU JJ, YIN CF, et al.Bacterial endotoxin test of mannose triflate[J]. Chemical Reagents(化学试剂), 2017, 39(9): 992-994.
[42] CHEN L, LIU XY, DU PF, et al.Establishment of quantitative detection method of bacterial endotoxin in docetaxel polymer micelles for injection[J]. China Pharmaceuticals(中国药业), 2022, 31(16): 61-64.
[43] ZHANG TT, LU L, DOU J, et al.Discussion on method employing chloroform as a solvent to detect bacterial endotoxin in omega-3-acid-triglycerides[J]. Chin J Pharm Anal(药物分析杂志), 2019, 39(2): 341-345.
[44] CHEN YL, JIN M.Study on the bacterial endotoxin test method for refined brucea javanica oil[J]. Evaluation and Analysis of Drug-Use in Hospitals of China(中国医院用药评价与分析), 2016, 16(1): 1-2.
[45] LIU H, XU LM.Comparative study on bacterial endotoxin test in progesterone injection[J]. Chin J Pharm Anal(药物分析杂志), 2014, 34(6): 1113-1119.
[46] WANG XR.Establishment of bacterial endotoxin test of metoclopramide raw material[J]. China Pharmacy(中国药房), 2014, 25(13): 1223-1224.
[47] Ministry of Health of the People’s Republic of China. Tachypleus Amebocyte Lysate departmental standard[S]. WS1-364(B-123)-91, 1991.
[48] BI H, GUO Y, LIU L, et al.Development of a method for bacterial endotoxin test on novel therapeutic gastric cancer vaccine[J]. Chin J Biologicals(中国生物制品学杂志), 2017, 30(9): 973-976.
[49] GENG X, NAN HY, FAN ZY, et al.Establishment of bacterial endotoxin test method for posaconazole raw material[J]. Food and Drug(食品与药品), 2022, 24(3): 278-281.