河鲀鱼基质中河豚毒素标准样品的研制  

Preparation of matrix reference material for tetrodotoxin in Tetraodontidae

作　　者：王伟 尹新颖 西日尼阿衣·阿里甫 徐敦明 肖晶 曹际娟 WANG Wei;YIN Xin-Ying;XIRINIAYI A-Li-Fu;XU Dun-Ming;XIAO Jing;CAO Ji-Juan(China National Center for Food Safety Risk Assessment,Beijing 100023,China;Key Laboratory of Biotechnology and Bioresources Utilization of Ministry of Education,Dalian Minzu University,Dalian 116600,China;Technology Center of Xiamen Customs District,Xiamen 361013,China)

机构地区：[1]国家食品安全风险评估中心,北京100023 [2]大连民族大学生物技术与资源利用教育部重点实验室,大连116600 [3]厦门海关技术中心,厦门361013

出　　处：《食品安全质量检测学报》2022年第5期1588-1596,共9页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2020YFF0305002);辽宁省“兴辽英才计划”项目(XLYC2002106)。

摘　　要：目的研制基于河鲀鱼基质的河豚毒素(tetrodotoxin,TTX)定量分析标准样品。方法以野生河鲀鱼肝脏、卵巢、精巢和肌肉组织为基料,利用正己烷脱脂分离处理后,经两次冷冻干燥制备河鲀鱼基质的TTX标准样品,采用液相色谱-串联质谱法进行定性确证。样品分装成500瓶后,进行均匀性、稳定性检验和定值分析。结果经确证该基体标准样品中含有TTX;从基体标准样品中随机抽取15瓶进行均匀性检验,经F检验表明在95%的置信区间范围内样品均匀性良好;长期稳定性考察在0~4℃低温条件下历经了长时间保存,短期稳定性在-80~55℃范围内进行运输条件下的考察,结果表明在考察期间内样品稳定性良好;经国内8家实验室进行协同定值,评定了定值结果的不确定度,该基体标准样品中TTX特性值及不确定度为(5.20±0.03)mg/kg(k=2)。结论该基体标准样品达到国家标准样品的技术要求,可用于对水产品中河豚毒素检测过程的方法验证与质量控制等活动。Objective To develop a matrix reference material for quantitative analysis of tetrodotoxin(TTX)based on Tetraodontidae matrix.Methods Based on puffer fish matrix,the liver,ovary,testis and muscle tissue of wild puffer fish were used as base materials,degreased and separated with n-hexane,and then freeze-dried twice to prepare the matrix reference material of TTX in Tetraodontidae,which was qualitatively confirmed by liquid chromatography-tandem mass spectrometry.After the sample was sub packed into 500 bottles,the uniformity,stability test and fixed value analysis were carried out.Results The matrix reference materia had been confirmed to contain TTX;15 bottles were randomly selected from the matrix reference material for uniformity test,and the F test showed that the sample uniformity was good within the confidence interval of 95%;the long-term stability was investigated under the low temperature of 0-4℃for a long time and the short-term stability was investigated under the transportation condition within the range of-80-55℃,the results showed that the stability of the samples were good during the investigation;the collaborative setting by 8 laboratories in China were conducted to assess the uncertainty of the calibration result,the TTX characteristic value and uncertainty of the matrix reference material were(5.20±0.03)mg/kg(k=2).Conclusion The matrix reference material meets the technical requirements of the national reference material,and can be used for method verification and quality control of TTX detection process in aquatic products.

关 键 词：河鲀鱼基质 河豚毒素 基体标准样品 制备 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]