[1]石骁昵,马宇熙,李 婷.UPLC-MS/MS法测定蔬菜中多菌灵含量的不确定度评估[J].医学信息,2020,33(03):162-164.[doi:10.3969/j.issn.1006-1959.2020.03.054]
　SHI Xiao-ni,LI Ting,MA Yu-xi.Evaluation of Uncertainty in Determination of Carbendazim in Vegetables by UPLC-MS/MS[J].Medical Information,2020,33(03):162-164.[doi:10.3969/j.issn.1006-1959.2020.03.054]
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UPLC-MS/MS法测定蔬菜中多菌灵含量的不确定度评估()
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医学信息[ISSN:1006-1959/CN:61-1278/R]

卷:
33卷
期数:
2020年03期
页码:
162-164
栏目:
诊疗技术
出版日期:
2020-02-01

文章信息/Info

Title:
Evaluation of Uncertainty in Determination of Carbendazim in Vegetables by UPLC-MS/MS
文章编号:
1006-1959（2020）03-0162-03
作者:
石骁昵; 马宇熙; 李 婷
（乌鲁木齐市疾病预防控制中心，乌鲁木齐 830026）
Author(s):
SHI Xiao-ni; LI Ting; MA Yu-xi
(Urumqi Center for Disease Control and Prevention,Urumqi 830026,Xinjiang,China)
关键词:
多菌灵; 蔬菜; 超高效液相色谱-质谱联用; 不确定度
Keywords:
Carbendazim; Vegetables; Ultra performance liquid chromatography-mass spectrometry;  Uncertainty
分类号:
Q450.7
DOI:
10.3969/j.issn.1006-1959.2020.03.054
文献标志码:
A
摘要:
目的 研究超高效液相色谱-质谱联用（UPLC-MS/MS）法测定蔬菜中多菌灵含量的不确定度。方法 色谱柱为Waters ACQUITY BEH C18,1.7μm，柱温：35℃；进样量5 μl；流动相：A为乙腈，B为0.05%甲酸水；流速：0.3 ml。梯度洗脱条件：0~5 min 30% A，70% B；5~6 min 95% A，5% B；6~7 min 30% A，70% B，采用多反应监测模式进行检测，对不确定来源进行分析，建立标准曲线模型，计算各变量的不确定度、合成不确定度、扩展不确定度。结果 超高效液相色谱-质谱联用法测定蔬菜中多菌灵含量的不确定度，影响最大的是标准溶液配制稀释过程中产生的不确定度。相对不确定度为0.233，在置信度为95%时，覆盖因子k=2，扩展不确定度为4.66%。结论 UPLC-MS/MS法测定多菌灵含量对测量不确定贡献最大的是标准溶液的配制和稀释过程中产生的不确定度，其次是标准曲线拟合时产生的不确定度。因此在实验过程中要严格操作规程，减少人为误差。
Abstract:
Objective To study the uncertainty of determination of carbendazim in vegetables by ultra performance liquid chromatography-mass spectrometry (UPLC-MS/MS). Methods The chromatographic column was Waters ACQUITY BEH C18, 1.7 μm, column temperature: 35 °C; injection volume was 5 μl; mobile phase: A was acetonitrile, B was 0.05% formic acid water; flow rate: 0.3 ml.Gradient elution conditions: 0~5 min 30% A, 70% B; 5~6 min 95% A, 5% B; 6~7 min 30% A, 70% B. Multi-reaction monitoring mode was used for detection. Analyze the sources of uncertainty, establish a standard curve model, and calculate the uncertainty, synthetic uncertainty, and expanded uncertainty of each variable.Results The uncertainty of the determination of carbendazim in vegetables by ultra performance liquid chromatography-mass spectrometry combined with the most significant factor was the uncertainty generated during the preparation and dilution of standard solutions. The relative uncertainty is 0.233.When the confidence is 95%, the coverage factor k=2 and the expanded uncertainty is 4.66%.Conclusion The most significant contribution to the measurement uncertainty of the determination of carbendazim by the UPLC-MS/MS method is the uncertainty generated during the preparation and dilution of the standard solution, followed by the uncertainty generated during the fitting of the standard curve. Therefore, it is necessary to strictly operate procedures during the experiment to reduce human error.

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更新日期/Last Update: 2020-02-01