目的 用氣相-質(zhì)譜聯(lián)用（GC-MS）法對(duì)維格列汀中氨基甲酸乙酯殘留的測(cè)定進(jìn)行不確定度評(píng)估。方法 結(jié)合氨基甲酸乙酯的實(shí)驗(yàn)方法，建立數(shù)學(xué)模型，對(duì)實(shí)驗(yàn)過程中供試品制備、對(duì)照品溶液的配制、樣品測(cè)量結(jié)果的重復(fù)性、樣品回收率中不確定度來源進(jìn)行分析。結(jié)果 GC-MS法測(cè)定維格列汀中氨基甲酸乙酯時(shí)，當(dāng)取樣量為200 mg，k=2（95%置信度），測(cè)量結(jié)果表述為：（2.423±0.069）mg/kg。供試品的制備、標(biāo)準(zhǔn)溶液配制過程、重復(fù)性、方法回收率對(duì)總的不確定度貢獻(xiàn)分別為10.33%、15.08%、56.88%、17.71%。結(jié)論 氨基甲酸乙酯在測(cè)定過程中，供試品制備、對(duì)照品溶液的配制、方法回收率對(duì)總的不確定度影響較小，樣品的重復(fù)測(cè)量是影響測(cè)量結(jié)果不確定度的主要來源，在實(shí)驗(yàn)過程中應(yīng)給予控制。

Objective To evaluate the uncertainty of measurement of ethyl carbamate residues by gas chromatography-mass spectroscopy (GC-MS). Methods To test the ethyl carbamate residues, a mathematical model was established. The preparation of test solution, preparation of reference solution, repeatability of sample measurement results and in sample recovery for the source of uncertainty were analyzed. Results when the amount of sample was 200 mg, k=2 (95% confidence), the result was expressed as:(2.423 ±0.069) mg/kg. The contribution of preparation of test sample, preparation process of standard solution, repeatability and method recovery to the total uncertainty was 10.33%, 15.08%, 56.88% and 17.71%, respectively. Conclusion Preparation of test solution, preparation of reference solution and sample recovery have little influence for the results, while the repeated measurement are the main factors affecting the uncertainty of the results of detection and analysis of ethyl carbamate residues, and should be given special attention and control during the experiment.

R927.2