高效液相色谱-光化学衍生法测定陈皮中黄曲霉毒素G2的不确定度评定
目的 评定高效液相色谱法-光化学衍生法测定陈皮中黄曲霉毒素G2的含量的不确定度。方法 参考中国药典四部通则2351黄曲霉毒素测定法第一法对陈皮进行提取, 以C18柱(4.6 mm×250 mm, 5 μm)为分析柱, 甲醇:乙腈:水(30:12:58, V:V:V)为流动相进行洗脱, 流速0.6 mL/min, 柱温40 ℃, 使用柱后光化学衍生器连接荧光检测器进行检测。找出影响不确定度的因素, 对不确定度进行评估, 并给出不确定度, 如实反映测量的置信度和准确度。结果 该批次陈皮样品中黄曲霉毒素G2的含量为0.08 μg/kg, 其实际含量可表示为(0.08±0.005) μg/kg (k=2)。结论 黄曲霉毒素G2测定过程中主要影响因素为高效液相色谱仪的校准, 其次为测量重复性, 而样品溶液的配置与对照品溶液的稀释引入的不确定因素较小, 天平称量引入的不确定因素可以忽略不计。
Objective To evaluate the uncertainty of determination of aflatoxin G2 in tangerine peel by high performance liquid chromatography-photochemical derivatization. Methods The extraction of dried tangerine peel was extracted with reference to the first method of the Chinese Pharmacopoeia, four general rules 2351, aflatoxin assay, using C18 column (4.6 mm×250 mm, 5 μm) as the analytical column, methanol: acetonitrile: water (30:12:58, V:V:V) elution as the mobile phase for gradient elution, the flow rate was 0.6 mL/min, and the column temperature was 40 °C. The fluorescence detector was connected with a post-column photochemical derivator for detection. The factors affecting the uncertainty were found out, the uncertainty was evaluated, and the uncertainty was given to accurately reflect the confidence and accuracy of the measurement. Results The content of aflatoxin G2 in this batch of tangerine peel samples was 0.08 g/kg, and the actual content could be expressed as (0.08±0.005) g/kg (k=2). Conclusion The main influencing factors in the determination process of aflatoxin G2 are the calibration of the high-performance liquid chromatography, followed by the measurement of repeatability, and the uncertainty factors of the sample solution configuration and the dilution introduction of the reference solution are less. The uncertainty introduced by the balance weighing is negligible.
标题：高效液相色谱-光化学衍生法测定陈皮中黄曲霉毒素G2的不确定度评定
英文标题：Evaluation of uncertainty in determination of aflatoxin G2 in tangerine peel by high performance liquid chromatography-photochemical derivatization
作者：
谢良山 上海佰年诗丹德检测技术有限公司
沈君子 上海佰年诗丹德检测技术有限公司
钱勇 上海诗丹德标准技术服务有限公司
中文关键词:高效液相色谱-光化学衍生法,陈皮,黄曲霉毒素G2,不确定度评定,
英文关键词:high performance liquid chromatography-photochemical derivatization,tangerine peel,aflatoxin,uncertainty evaluation,
发表日期：2019-03-28
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