重复性测定结果可接受性检查方法在高效液相法色谱法含量测定中的应用
|
摘要
目的:根据我国国家标准,建立药物含量测定高效液相色谱法重复性测定结果可接受性检查的一般流程。方法:设计了实验室内小型实验方案,通过统计学方法推导出重复性限。从而计算得到相应方法的可接受性限。结果:高效液相色谱法进行药物含量测定的重复性限为r=3.44。结论:通过实验室内部数据的采集,评估重复性限,建立药物含量测定高效液相色谱法重复性测定结果可接受性检查的方法,为完善《中国药典》中方法重复性的要求提供了依据。
Objective: To establish a general process of acceptable assessment method of the repeatability test results in high perform ance liquid chrom atography for drug assay according to C hina National Standard. M ethods: Based on an internal analytical lab experiment,a repeatable limit was calculated by statistical method,then an acceptable assessm ent m ethod w as proposed. Results: The value of the repeatable lim it for determ ination of assay by high perform ance liquid chrom atography w as 3. 4 4 approxim ately. Conclusion : A general acceptable assessm ent m ethod of the repeatability test results in high perform ance liquid chrom atography for assay is established. That provides the scientific support to im prove the requirem ents on the repeatability in C hinese Pharm acopoeia.
Objective: To establish a general process of acceptable assessment method of the repeatability test results in high perform ance liquid chrom atography for drug assay according to C hina National Standard. M ethods: Based on an internal analytical lab experiment,a repeatable limit was calculated by statistical method,then an acceptable assessm ent m ethod w as proposed. Results: The value of the repeatable lim it for determ ination of assay by high perform ance liquid chrom atography w as 3. 4 4 approxim ately. Conclusion : A general acceptable assessm ent m ethod of the repeatability test results in high perform ance liquid chrom atography for assay is established. That provides the scientific support to im prove the requirem ents on the repeatability in C hinese Pharm acopoeia.
引文
[1]GB/T6379.6-2009测量方法与结果的准确度(正确度与精密度)第6部分:准确度值的实际应用[S].2009GB/T6379.6-2009 Accuracy(trueness and precision)of measurement methods and results-Part 6:Use in practice of accuracy values[S].2009
[2]GB/T11792-89测试方法的精密度在重复性或再现性条件下所得测试结果可接受性检査和最终测试结果的确定[S].1989GB/T11792-89 Precision of test methods-Check the acceptability of test results obtained under repeatability and reproducibility conditions and to determine final test results[S].1989
[3]GB/T601-2002化学试剂标准滴定溶液的制备[S].2002BG/T601-2002 Chemical reagent-Preparations of standard columetric solutions[S].2002
[4]中国药品生物制品检定所,中国药品检验总所.中国药品检验标准操作规范[M].北京:中国医药科技出版社,2010National Institutes for Food and Drug Control.China drug inspection operation standard[M].Beijing:China Medical Science Press,2010
[5]王林波,刘蔚,李苗,等.重复性测定结果可接受性检查方法在滴定液标定中的应用[J].中国药品标准,2015,16(3):172WANG LB,LIU W,LI M.et al.Application of acceptable assessment method of test results under repeatability conditions in standard volumetric solution standardization[J].Drug Stand China,2015,16(3):172
[6]中国药典2015版.四部[S].2015:374Ch P[S].2015 VolⅣ:374
[7]GB/T6379.2-2004测量方法与结果的准确度(正确度与精密度)第2部分:确定标准测量方法重复性和再现性的基本方法[S].2004GB/T6379.2-2004 Accuracy(trueness and precision)of measurement methods and results-Part 2:basic method for the determination of repeatability and reproducibility of a standard measurement method[S].2004
[2]GB/T11792-89测试方法的精密度在重复性或再现性条件下所得测试结果可接受性检査和最终测试结果的确定[S].1989GB/T11792-89 Precision of test methods-Check the acceptability of test results obtained under repeatability and reproducibility conditions and to determine final test results[S].1989
[3]GB/T601-2002化学试剂标准滴定溶液的制备[S].2002BG/T601-2002 Chemical reagent-Preparations of standard columetric solutions[S].2002
[4]中国药品生物制品检定所,中国药品检验总所.中国药品检验标准操作规范[M].北京:中国医药科技出版社,2010National Institutes for Food and Drug Control.China drug inspection operation standard[M].Beijing:China Medical Science Press,2010
[5]王林波,刘蔚,李苗,等.重复性测定结果可接受性检查方法在滴定液标定中的应用[J].中国药品标准,2015,16(3):172WANG LB,LIU W,LI M.et al.Application of acceptable assessment method of test results under repeatability conditions in standard volumetric solution standardization[J].Drug Stand China,2015,16(3):172
[6]中国药典2015版.四部[S].2015:374Ch P[S].2015 VolⅣ:374
[7]GB/T6379.2-2004测量方法与结果的准确度(正确度与精密度)第2部分:确定标准测量方法重复性和再现性的基本方法[S].2004GB/T6379.2-2004 Accuracy(trueness and precision)of measurement methods and results-Part 2:basic method for the determination of repeatability and reproducibility of a standard measurement method[S].2004