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为了比较液相色谱串联质谱采用内标法与外标法的不同,试验采用牛奶样品经甲醇-水溶液提取,过免疫亲和柱净化和富集后,液相色谱串联质谱法进行检测,分别用同位素内标法、目前平台已建立的外标法进行定量分析。结果表明:采用同位素内标法,黄曲霉素M1在0.05～5ng/mL范围内线性相关系数为0.9992,检出限为0.005μg/kg,定量限为0.015μg/kg;采用外标法定量,黄曲霉素M1在0.1～10ng/mL范围内线性相关系数为0.9994,检出限为0.002μg/kg,定量限为0.005μg/kg。在0.1～1ng/mL加标浓度范围内,内标法的回收率在89.9%～104.7%之间,相对标准偏差(RSD)不大于5.2%;而外标法的回收率在81.0%～107.5%之间,RSD不大于9.0%。说明检测生鲜乳中黄曲霉素M1时,内标法的准确度和精密度均优于外标法,但检测结果差异不显著(P>0.05)。采用内标法和外标法定量分析结果均能满足检测要求,检测人员可根据实验室实际情况选择合适的定量方法。
In order to compare the difference between internal standard method and external standard method in liquid chromatography tandem mass spectrometry, the milk samples were extracted by methanol-water solution, purified by immunoaffinity column and enriched by liquid chromatography-tandem mass spectrometry Isotope internal standard method, the current platform has been established by external standard method for quantitative analysis. The results showed that the linear correlation coefficient of aflatoxin M1 in the range of 0.05 ~ 5ng / mL was 0.9992 with the detection limit of 0.005μg / kg and the limit of quantification of 0.015μg / kg using isotope internal standard method. The external standard method was used to quantify The linear correlation coefficient of aflatoxin M1 in the range of 0.1 ~ 10ng / mL was 0.9994, the detection limit was 0.002μg / kg and the limit of quantification was 0.005μg / kg. The recoveries of the internal standard method ranged from 89.9% to 104.7% and the relative standard deviations (RSDs) were no more than 5.2% at the spiked concentration range of 0.1 ~ 1ng / mL, while the recoveries of the external standard method ranged from 81.0% to 107.5% %, RSD not more than 9.0%. The results showed that the accuracy and precision of internal standard method were better than external standard method when detecting aflatoxin M1 in raw milk, but the difference was not significant (P> 0.05). The internal standard method and external standard method can meet the requirements of quantitative analysis of quantitative analysis, testing staff can choose the appropriate laboratory quantitative methods.