| GC－NCI－MS衍生化法同时测定全血中的亚硝酸根和硝酸根 |
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| 基金项目:中央级基本科研业务费资助（2020JB011） |
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| 中文摘要:建立了全血中亚硝酸根（NO?22-）和硝酸根（NO?33-）的衍生化气相色谱－负化学电离源－质谱（GC－NCI－MS）定量分析方法。以同位素标记的15NO?22-和15NO?33-为内标，将全血中的NO?22-和NO?33-提取衍生后，对目标衍生物进行GC－NCI－MS分析。优化了目标物提取溶剂、衍生物提取溶剂、相转移试剂用量、衍生化方式、衍生化反应时间和温度，确定了最佳前处理条件。结果表明，全血中NO?22-在0.05～5 μg/mL范围内线性关系良好（r2 = 0.995），检出限为0.01 μg/mL，准确度为89.6%～98.0%，日内和日间相对标准偏差（RSD）分别为1.8%～9.2%和2.1%～6.2%，提取回收率为99.8%～118%；NO?33-在1～300 μg/mL范围内线性关系良好（r2 = 0.997），检出限为0.2 μg/mL，准确度为92.8%～112%，日内和日间RSD分别为0.60%～14%和0.60%～3.7%，提取回收率为80.3%～88.4%。应用该方法测得16份健康人体全血中内源性NO?22-和NO?33-的质量浓度分别为0.05～0.10 μg/mL和1.70～7.70 μg/mL。对真实亚硝酸盐中毒人体的全血进行测定，2种目标物的质量浓度远高于人体全血中内源性的浓度水平，可判定为亚硝酸盐中毒。该方法特异性强、灵敏度高，结果准确、可靠，能够满足亚硝酸盐中毒案件的检验鉴定需求。 |
| 中文关键词:亚硝酸根 ?硝酸根 ?全血 ?气相色谱－负化学电离源－质谱（GC－NCI－MS） ?毒物分析 |
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| Simultaneous Determination of Nitrite and Nitrate in Whole Blood by GC－NCI－MS with Derivatization |
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| Abstract:A gas chromatography－negative chemical ionization－mass spectrometry（GC－NCI－MS） with derivatization was developed for the quantitative analysis of nitrite（NO?22-） and nitrate（NO?33-） in whole blood. Isotope-labeled?15NO?22- and 15NO?33- were used as the internal standards．After NO?22- and NO?33- in whole blood were extracted and derivatized，the target derivatives were analyzed by GC－NCI－MS. The target extraction solvent，derivative extraction solvent，amount of phase transfer reagent，the derivatization method，time and temperature of the derivatization reaction were optimized．The optimal pretreatment conditions were also determined．A negative chemical ionization source（NCI） was used to select ion monitor（SIM）．The quantitative ions for target NO?22- and its internal standard 15NO?22- were m/z 46 and 47，while those for target NO?33- and its internal standard 15NO?33- were m/z 62 and 63，respectively．There was a good linear relationship for NO?22- in whole blood（r2 = 0.995） in the range of 0.05－5 μg/mL，with a detection limit of 0.01 μg/mL and an accuracy of 89.6%－98.0%．The extraction recoveries ranged from 99.8% to 118%，with the intra-day and inter-day relative standard deviations（RSDs） of 1.8%－9.2% and 2.1%－6.2%，respectively．There also existed a good linear relationship for NO?33- in whole blood（r2 = 0.997） in the range of 1－300 μg/mL，with a detection limit of 0.2 μg/mL and an accuracy of 92.8%－112%．The extraction recoveries ranged from 80.3% to 88.4%，with the intra-day and inter-day RSDs of 0.60%－14% and 0.60%－3.7%，respectively. The endogenous NO?22- and NO?33- in 16 whole blood samples of healthy person were determined by this method．The results showed that the concentrations of NO?22- and NO?33- were in the ranges of 0.05－0.10 μg/mL and 1.70－7.70 μg/mL，respectively．In addition，the contents of two target substances in real human whole blood poisoned by nitrite were determined，and the concentrations of both substances were much higher than the endogenous concentration level in whole blood of human body，thus nitrite poisoning was determined．With the advantages of strong specificity，high sensitivity，accuracy and reliability，the method could meet the requirements for inspection and identification of nitrite poison cases． |
| Key Words:nitrite ?nitrate ?whole blood ?gas chromatography－negative chemical ionization－mass spectrometry（GC－NCI－MS） ?toxicological analysis |
| 引用本文：崔婉莹，赵鹏，饶渝兰，于忠山，张云峰，董林沛，魏春明，吴小军.GC－NCI－MS衍生化法同时测定全血中的亚硝酸根和硝酸根[J].分析测试学报,2022,41(5):781-786. |
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