摘要
为提升稻米中黄曲霉毒素B_(1)(AFTB_(1))检测的实验室内部质量控制水平,按照GB 5009.22—2016《食品安全国家标准食品中黄曲霉毒素B族和G族的测定》第三法和AFTB_(1)免疫亲和柱操作说明书,建立高效液相色谱-柱后光化学衍生法测定稻米中AFTB_(1)含量的方法,通过标准曲线制作、精密度试验、回收率试验、人员比对试验等质量控制手段对测定结果进行评价,并对其试验前处理操作关键点进行分析。结果表明,AFTB_(1)在0.5~40 ng/mL的范围内线性关系良好,相关系数>0.9999,方法检出限和定量限分别为0.03、0.1μg/kg;方法定性数据(保留时间)和定量数据(峰面积)的相对标准偏差分别为0.06%、0.10%;在5、10、20μg/kg加标水平下,3个浓度水平回收率为95.3%~100.6%,相对标准偏差≤1.7%;15名检测人员随机选取2个浓度的AFTB_(1)质控样品,其测定双试验结果相对标准偏差均≤4.4%,Z比分数评价均满足|Z|≤1,表明“优秀”。人员比对试验既可作为评估检测人员操作技能与专业水平的有效手段,又可为实验室质量管理及质量控制提供重要数据保障。
To enhance the internal quality control level within the laboratory for the detection of aflatoxin B_(1)(AFTB_(1))in rice,a method for determining AFTB_(1)content in rice was established by using high-performance liquid chromatography(HPLC)with post-column photochemical derivation,in accordance with the third method of National Food Safety Standard-Determination of Aflatoxin B and G in Foods(GB 5009.22—2016)and the operation manual of the AFTB_(1)immunoaffinity column.The determination results were evaluated through quality control measures such as standard curve making,precision test,recovery test,and personnel comparison test,and the key points of pre-treatment operation before the test were analyzed.The results showed that AFTB_(1)exhibited a good linear relationship within the range of 0.5-40 ng/mL,with all correlation coefficients>0.9999.The detection limit and quantification limit of the method were 0.03μg/kg and 0.1μg/kg,respectively.The relative standard deviations for qualitative data(retention time)and quantitative data(peak area)were 0.06%and 0.10%,respectively.At spiked levels of 5μg/kg,10μg/kg,and 20μg/kg,the recovery rates at the three concentration levels ranged from 95.3%to 100.6%,with relative standard deviations≤1.7%.For 15 testing personnel randomly selecting two concentrations of AFTB_(1)quality control samples,the relative standard deviations of the dual-test results were≤4.4%,and the Z-score evaluations all showed|Z|≤1,indicating"excellent"performance.Personnel comparison tests can serve as an effective means to evaluate the operational skills and professional level of testing personnel,and also provide important data support for the quality management and quality control of the laboratory.
作者
严虹
YAN Hong(Hunan Provincial Center for Monitoring of Grain and Oil Products Quality//National Engineering Laboratory for Deep Processing of Rice and Byproducts,Changsha 410201,China)
出处
《粮食与饲料工业》
2025年第6期115-119,共5页
Cereal & Feed Industry
基金
2025年“湖南优质粮油工程升级版”项目(湘粮产[2025]38号)。
