赵静,段建华,白艳梅*,刘丽君,李翠枝,吴晓莉,吕志勇
[内蒙古伊利实业集团股份有限公司,国家市场监管重点实验室(乳及乳制品检测与监控技术),内蒙古 呼和浩特 010110]
摘要:应用Minitab 软件,优化液相色谱-串联质谱测定牛乳中氟氢可的松方法的参数条件。利用Minitab 软件中单因素方差分析、实验设计(Design of experiment,DOE)等工具,研究称样量、提取试剂、复溶试剂、洗脱试剂对回收率的影响,确定最优的检测条件。结果表明,优化参数条件后,添加水平分别为0.4、0.8、4μg/kg 时,回收率达到72.3%~109.3%,相对标准偏差达到6.7%~12.0%,满足方法学验证要求。通过应用Minitab 软件,可以准确找到影响检测结果的关键影响因子及最佳参数条件,为检测方法优化提供科学依据,从而保证检测结果更加准确、可靠。
关键词:Minitab 软件;牛乳;氟氢可的松;液相色谱-串联质谱
Minitab Software in Fludrocortisone Detection Method Application of Optimization
ZHAO Jing,DUAN Jian-hua,BAI Yan-mei*,LIU Li-jun,LI Cui-zhi,WU Xiao-li,LV Zhi-yong
(Inner Mongolia Yili Industrial Group Co.,Ltd.,Key Laboratory of Milk and Dairy Products Detection and MonitoringTechnology for
State Market Regulation,Hohhot 010110,China)
Abstract: Minitab software was used to optimize the parameter conditions of determination of fludrocortisone in milkby liquid chromatography-tandem mass spectrometry. Using Minitab software,one-way ANOVA and DOE experimentaldesign were carried out. The effects of sample weighing,extraction reagent,redissolution reagent and elution reagenton recovery rate were studied,and the optimal detection conditions were determined. The results showed that afteroptimizing the parameter conditions,when the addition levels were 0.4,0.8 and 4μg/kg,the recovery rate reached72.3% ~109.3% ,and the relative standard deviation reached 6.7% ~12.0% ,which met the requirements ofmethodology verification. By using Minitab software,we can accurately find the key influencing factors and the bestparameter conditions that affect the detection results,and provide scientific basis for the optimization of detectionmethods,so as to ensure that the detection results are more accurate and reliable.
Key words: minitab software;milk;fludrocortisone;liquid chromatography-tanden mass spectrometry(LC-MS/MS)
中图分类号:TS252.7 文献标志码:A 文章编号:1007-7871(2023)05-0010-07
2023,Vol.26,No.5