两种螨变应原注射液氯化钠含量检测方法的比较
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摘要
目的验证电位滴定法用于螨变应原注射液氯化钠含量测定的可行性。方法利用电位滴定法和硫氰酸铵滴定法检测螨变应原注射液中氯化钠含量,确定两种方法的线性范围,并进行精密性、准确性验证。应用两种方法测定13批螨变应原注射液中氯化钠含量。结果电位滴定法测定螨变应原注射液氯化钠含量的线性检测范围(0.10~1.50 m L)较硫氰酸铵滴定法(0.50~1.50 m L)广;精密性验证结果表明,电位滴定法检测氯化钠含量的RSD不高于1.87%,硫氰酸铵滴定法不高于1.97%;准确性验证结果表明,硫氰酸铵滴定法检测氯化钠含量的加标回收率为95.20%~112.66%,电位滴定法为92.88%~99.44%。两种方法检测13批(共27个亚批)螨变应原注射液氯化钠含量,结果基本一致,差异无统计学意义(P>0.05),且全部符合该制品注册检验标准。结论电位滴定法可作为硫氰酸铵滴定法的补充方法,用于螨变应原注射液氯化钠含量的测定。
Objective To validate the feasibility of determination of sodium chloride content in mite allergen injection by potentiometric titration method. Methods The sodium chloride content in mite allergen injection was determined by potentiometric titration and ammonium thiocyanate titration respectively. The linear ranges of the two methods were determined,while the precisions and accuracies were validated. The sodium chloride contents in 30 batches of mite allergen injection were determined by the two methods,and the results were compared and analyzed. Results The linear range of potentiometric titration(0. 10 ~ 1. 50 m L) was larger than that of ammonium thiocyanate titration(0. 50 ~1. 50 m L). The RSD of determination result of sodium chloride content by potentiometric titration was not more than1. 87%,while that by ammonium thiocyanate titration was not more than 1. 97%. The recovery rate of sodium chloride content in accuracy validation of ammonium thiocyanate titration was 95. 20% ~ 112. 66%,while that of potentiometric titration was 92. 88% ~ 99. 44%. However,the determination results of sodium chloride contents in 13 batches(27 subbatches) of mite allergen injection by the two methods were basically in agreement(P > 0. 05),which met the requirements for license of the product. Conclusion As a supplementary method for ammonium thiocyanate titration,potentiometric titration may be used for the determination of sodium chloride content in mite allergen injection.
Objective To validate the feasibility of determination of sodium chloride content in mite allergen injection by potentiometric titration method. Methods The sodium chloride content in mite allergen injection was determined by potentiometric titration and ammonium thiocyanate titration respectively. The linear ranges of the two methods were determined,while the precisions and accuracies were validated. The sodium chloride contents in 30 batches of mite allergen injection were determined by the two methods,and the results were compared and analyzed. Results The linear range of potentiometric titration(0. 10 ~ 1. 50 m L) was larger than that of ammonium thiocyanate titration(0. 50 ~1. 50 m L). The RSD of determination result of sodium chloride content by potentiometric titration was not more than1. 87%,while that by ammonium thiocyanate titration was not more than 1. 97%. The recovery rate of sodium chloride content in accuracy validation of ammonium thiocyanate titration was 95. 20% ~ 112. 66%,while that of potentiometric titration was 92. 88% ~ 99. 44%. However,the determination results of sodium chloride contents in 13 batches(27 subbatches) of mite allergen injection by the two methods were basically in agreement(P > 0. 05),which met the requirements for license of the product. Conclusion As a supplementary method for ammonium thiocyanate titration,potentiometric titration may be used for the determination of sodium chloride content in mite allergen injection.
引文
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[10]CHENG Y F,WANG G H,YAN X L,et al.Potentiometric titration determination of sodium chloride in clindamycin phosphate and sodium chloride injection[J].Anhui Med Pharm J,2005,9(1):40-41.(in Chinese)程云峰,王光华,宛小林,等.电位滴定法测定克林霉素磷酸酯氯化钠注射液中氯化钠含量[J].安徽医药,2005,9(1):40-41.
[11]YU L Y,HU C J,HUANG Q W,et al.Determine the contents of sodium chloride in the fructus psoraleae[J].J Chengdu Med Coll,2009,4(2):83-85.(in Chinese)余凌英,胡昌江,黄勤挽,等.电位滴定法测定盐炙补骨脂中氯化钠含量[J].成都医学院学报,2009,4(2):83-85.
[2]FERNANDEZ-CALDAS E.Towards a more complete standardization of mite allergen extracts[J].Int Arch Allergy Immunol,2013,160(1):1-3.
[3]PARK K H,SON M,CHOI S Y,et al.In vitro evaluation of allergen potencies of commercial house dust mite sublingual immunotherapy reagents[J].Allergy Asthma Immunol Res,2015,7(2):124-129.
[4]CARNES J,IRAOLA V,CHO S H,et al.Mite allergen extracts and clinical practice[J].Ann Allergy Asthma Immunol,2017,118(3):249-256.
[5]SPIRIC J,REUTER A,RABIN R L.Mass spectrometry to complement standardization of house dust mite and other complex allergenic extracts[J].Clin Exp Allergy,2017,47(5):604-617.
[6]NOLTE H,PLUNKETT G,GROSCH K,et al.Major allergen content consistency of SQ house dust mite sublingual immunotherapy tablets and relevance across geographic regions[J].Ann Allergy Asthma Immunol,2016,117(3):298-303.
[7]Chinese Pharmacopoeia Commission.Pharmacopoeia of People's Repubic of China(VolⅢ)[S].Beijing:China Med Sci Press,2015:General Rule 55.(in Chinese)国家药典委员会.中国药典(三部)[S].北京:中国医药科技出版社,2015:通则55.
[8]Chinese Pharmacopoeia Commission.Pharmacopoeia of People's Repubic of China(VolⅤ)[S].Beijing:China Med Sci Press,2015:86-87.(in Chinese)国家药典委员会.中国药典(四部)[S].北京:中国医药科技出版社,2015:86-87.
[9]李晓强,祝晓凤.自动滴定法与手动滴定法测定药品含量的差异性研究[J].世界最新医学信息文摘,2017,17(14):172-174.
[10]CHENG Y F,WANG G H,YAN X L,et al.Potentiometric titration determination of sodium chloride in clindamycin phosphate and sodium chloride injection[J].Anhui Med Pharm J,2005,9(1):40-41.(in Chinese)程云峰,王光华,宛小林,等.电位滴定法测定克林霉素磷酸酯氯化钠注射液中氯化钠含量[J].安徽医药,2005,9(1):40-41.
[11]YU L Y,HU C J,HUANG Q W,et al.Determine the contents of sodium chloride in the fructus psoraleae[J].J Chengdu Med Coll,2009,4(2):83-85.(in Chinese)余凌英,胡昌江,黄勤挽,等.电位滴定法测定盐炙补骨脂中氯化钠含量[J].成都医学院学报,2009,4(2):83-85.