国家药品对照品有机氯农药混合对照品溶液的研制与不确定度评定

目的：制备适用于中国药典2015年版农药残留量测定法的农药标准物质。方法：以药典通则2341中规定的22种农药为研究对象，以农药标准物质为原料，用容量法制备，采用气相色谱-电子捕获检测法（GC-ECD法）进行均匀性和稳定性检验，协作标定进行定值，并对量值的不确定度进行评估。结果：22种农药的质量浓度范围为9.9~10.5 μg·mL^-1，相对扩展不确定度为2.8%~8.4%。结论：有机氯农药混合对照品溶液符合国家药品对照品的技术要求，可为药品检验、科学研究等方面的测量和研究工作提供技术支撑和量值溯源保障。

Objective:To prepare pesticide reference substance for the determination of pesticide residues following Chinese Pharmacopoeia(ChP)of 2015 edition.Method:22 kinds of pesticides described in the general rules 2341 of ChP were selected as the research objects.With the reference materials as raw material,mixed reference solution of organochlorine pesticide was prepared by volumetric method.After the homogeneity and stability tested by the gas chromatograph with configuring electron capture detector(GC-ECD),collaborative calibration was used to set the value and the uncertainty of the fixed value was evaluated.Results:The mass concentration of 22 pesticides ranged from 9.9 to 10.5 μg·mL^-1,and the relative expanded uncertainty was 2.8%-8.4%.Conclusion:Mixed reference solution of organochlorine pesticide met the technical requirements of the national reference substance,and provided technical support for the measurement and research work in the field of drug control and scientific research.

[1] 中国药典2015年版.四部[S].2015:209 ChP 2015.Vol Ⅳ[S].2015:209
[2] JJF1343-2012标准物质定值的通用原则及统计学原理[S].2012:5 JJF1343-2012 General and Statistical Principles for Characterization of Reference Materials[S].2012:5
[3] CNAS-GL29标准物质/标准样品定值的一般原则和统计方法[S].2010 CNAS-GL29.Reference materials-General and statistical Principles for Certification[S].2010
[4] JJF 1135-2005化学分析测量不确定度评定[S].2005 JJF1135-2005 Evaluation of Uncertainty in Chemical Analysis Measurement[S].2005
[5] JJG196-2006常用玻璃量器[S].2006 JJG196-2006 Working Class Container[S].2006
[6] CNAS-GL06.化学分析中不确定度的评估指南[S].2006 CNAS-GL06.Guidance on Evaluating the Uncertainty in Chemical Analysis CNAS[S].2006
[7] 徐华能.多菌灵农药标准物质的研制[J].农药,2012,51(3):190 XU HN.Preparationof reference material of carbendazim[J].Chin J Pestic,2012,51(3):190
[8] 王璐,彭袆,罗铭.六氯苯·马拉硫磷和治螟磷标准工作液的研制与不确定度评定[J].安徽农业科学,2014,42(27):9344 WANG L,PENG H,LUO M.Preparation and uncertainty evaluation on standard work-solution of hexachl,orobenzene,malathion and sulfotep[J].J Anhui Agric Sci,2014,42(27):9344
[9] 邵明武,汤桦,陈大舟.关于多组分痕量有机污染物溶液标准物质研制的体会[J].计量技术,2007,12(3):61 SHAO MW,TANG H,CHEN DZ.The experience about manufacturing standard substance solution of multicomponent trace organic pollutans[J].Measur Technol,2007,12(3):61
[10] GONG NB,WANG XY,ZHANG BX,et al.Characterization and uncertainty evaluation of a new certified reference material of baicalein[J].J Pharm Biomed Anal,2014,89(2):106
[11] 马玲云,陈红岩,肖新月,等.标示量值七叶皂苷对照提取物的研制[J].药物分析杂志,2014,34(7):1278 MA LY,CHEN HY,XIAO XY,et al.Preparation of aescinate extractive reference standard at labeled amounts[J].Chin J Pharm Anal,2014,34(7):1278
[12] 常艳,马双成,胡昌勤.美洛西林标准物质短期稳定性研究[J].药物分析杂志,2013,33(4):684 CHANG Y,MA SC,HU CQ.Short-term stability study of mezlocillin reference material[J].Chin J Pharm Anal,2013,33(4):684
[13] 何风艳,戴忠,何轶,等.西红花苷对照提取物的定值及不确定度评估研究[J].药物分析杂志,2016,36(6):1113 HE FY,DAI Z,HE Y,et al.Certification and uncertainty evaluation of crocin reference extract[J].Chin J Pharm Anal,2016,36(6):1113
[14] 卢宪波,陈吉平,王淑秋,等.贻贝中有机氯农药和多氯联苯标准物质的研制及同位素稀释高分辨质谱法定值[J].色谱,2012,30(9):915 LU XB,CHEN JP,WANG SQ,et al.Preparation and certification of mussel reference material for organochlorine pesticides and polychlorinated biphenyls using isotope ilution-high resolution mass spectrometry[J].Chin J Chromatogr,2012,30(9):915