液相色谱-串联质谱法检测对虾中T-2毒素的 不确定度评定
目的 评定液相色谱-串联质谱检测对虾中T-2毒素的不确定度。方法 样品经乙酸乙酯提取, 无水硫酸钠脱水, 提取上清液氮气吹干后用1 mL 0.1%甲酸的甲醇:水溶液(3:7, V:V)定容, 正己烷除脂。基质匹配法定量。液相采用甲醇和0.1%甲酸酸化的5 mmol/L乙酸铵溶液梯度洗脱, 质谱采用电喷雾离子化方式下正离子的选择离子监测模式对T-2毒素的定量离子和定性离子进行监测。通过分析并计算检测过程中各不确定度分量得到合成标准不确定度。结果 本方法检测T-2毒素的合成标准不确定度为0.739 μg/kg, 取置信概率95%的扩展不确定度为1.5 μg/kg。所以, 试样中T-2毒素的测量结果为: X=(12.7±1.5) μg/kg, k=2。结论 此检测方法使外标法的定量结果更为真实有效, 方法不确定度的评定亦可为采用空白基质匹配法的现行相关检测方法的不确定度评估提供参考。
Objective To evaluate the uncertainty of T-2 toxin determination in prawns by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were extracted by ethyl acetate, dehydrated by sodium sulfate, concentrated upper layer by nitrogen, dissolved by 1 mL 0.1% formic acid in methyl alcohol:water (3:7, V:V), and degreased by hexane. The target compounds were quantified by matrix-matched calibration standard. The T-2 toxin was separated on a reversed phase using a gradient elution program of 0.1% formic acid methyl alcoholsolution and 0.1% formic acid in 5 mmol/L ammonium acetate. LC–MS/MS with selected reactions monitoring (SRM) was used, and the T-2 toxin was identified based upon the intensities of fragments. Then the combined standard uncertainty was determined by analyzing and calculating various measurements of uncertainties. Results The relative combined standard uncertainty of this method was 0.739 μg/kg. The expanded uncertainty was 1.5 μg/kg when the fiducial probability was about 95%. So the measurement result of T-2 toxin in the sample was (12.7±1.5) μg/kg, k=2. Conclusion This detection method makes the results of external standard method more realistic and effective. The evaluation method of measurement uncertainty in this article can also provide a reference for the correlation detection method which quantified by matrix-matched calibration standard.
标题：液相色谱-串联质谱法检测对虾中T-2毒素的 不确定度评定
英文标题：Uncertainty evaluation of T-2 toxin determination in prawns by liquid chromatography-tandem mass spectrometry
作者：
施琦 广东省湛江市质量计量监督检测所,国家海产品质量监督检验中心(湛江)
刘阳 广东省湛江市质量计量监督检测所,国家海产品质量监督检验中心(湛江)
王雅玲 广东海洋大学食品科技学院,广东省水产品加工与安全重点实验室,广东普通高等学校水产品深加工重点实验室
孔冬伟 广东省湛江市质量计量监督检测所,国家海产品质量监督检验中心(湛江)
杨嘉丽 广东省湛江市质量计量监督检测所,国家海产品质量监督检验中心(湛江)
雷大明 广东省湛江市质量计量监督检测所,国家海产品质量监督检验中心(湛江)
孙力军 广东海洋大学食品科技学院,广东省水产品加工与安全重点实验室,广东普通高等学校水产品深加工重点实验室
毕思远 深圳市通量检测科技有限公司,深圳市易瑞生物技术有限公司
中文关键词:T-2毒素,液相色谱质谱联用法,对虾,不确定度,
英文关键词:T-2 toxin,liquid chromatography-tandem mass spectrometry,prawn,uncertainty,
发表日期：2016-03-17
- 文件大小:
- 293.47 KB
- 下载次数:
- 60
-
高速下载
|
|
