Simultaneous Determination of Nitrite and Nitrate in Whole Blood by GC－NCI－MS with Derivatization

CUI Wan-ying; ZHAO Peng; RAO Yu-lan; YU Zhong-shan; ZHANG Yun-feng; DONG Lin-pei; WEI Chun-ming; WU Xiao-jun

doi:10.19969/j.fxcsxb.21070601

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Simultaneous Determination of Nitrite and Nitrate in Whole Blood by GC－NCI－MS with Derivatization

Experimental Techniques and Methods | 更新时间：2022-06-22

- Simultaneous Determination of Nitrite and Nitrate in Whole Blood by GC－NCI－MS with Derivatization
- Journal of Instrumental Analysis Vol. 41, Issue 5, Pages: 781-786(2022)
- 作者机构：
  
  1.中国人民公安大学侦查学院，北京 100038
  2.公安部物证鉴定中心，北京 100038
  3.复旦大学基础医学院，上海 200032
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21070601
  CLC：
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崔婉莹,赵鹏,饶渝兰等.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(05):781-786.

CUI Wan-ying,ZHAO Peng,RAO Yu-lan,et al.Simultaneous Determination of Nitrite and Nitrate in Whole Blood by GC－NCI－MS with Derivatization[J].Journal of Instrumental Analysis,2022,41(05):781-786.
崔婉莹,赵鹏,饶渝兰等.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(05):781-786. DOI： 10.19969/j.fxcsxb.21070601.

CUI Wan-ying,ZHAO Peng,RAO Yu-lan,et al.Simultaneous Determination of Nitrite and Nitrate in Whole Blood by GC－NCI－MS with Derivatization[J].Journal of Instrumental Analysis,2022,41(05):781-786. DOI： 10.19969/j.fxcsxb.21070601.

摘要

建立了全血中亚硝酸根（NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248025&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248023&type=,1.10066664,3.72533321,）和硝酸根（NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248082&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248081&type=,1.10066664,3.72533321,）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,15,NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248093&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248092&type=,1.10066664,3.72533321,和,15,NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248063&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248061&type=,1.10066664,3.72533321,为内标，将全血中的NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248046&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248043&type=,1.10066664,3.72533321,和NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248050&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248048&type=,1.10066664,3.72533321,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, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248098&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248095&type=,1.10066664,3.72533321,在0.05～5 μg/mL范围内线性关系良好（,r,2, = 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, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248058&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248057&type=,1.10066664,3.72533321,在1～300 μg/mL范围内线性关系良好（,r,2, = 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, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248060&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248059&type=,1.10066664,3.72533321,和NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248063&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248061&type=,1.10066664,3.72533321,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。

Abstract

A gas chromatography－negative chemical ionization－mass spectrometry（GC－NCI－MS） with derivatization was developed for the quantitative analysis of nitrite（NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248093&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248092&type=,1.10066664,3.72533321,） and nitrate（NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248103&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248100&type=,1.10066664,3.72533321,） in whole blood. Isotope-labeled ,15,NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248093&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248092&type=,1.10066664,3.72533321, and ,15,NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248082&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248081&type=,1.10066664,3.72533321, were used as the internal standards．After NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248093&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248092&type=,1.10066664,3.72533321, and NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248090&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248089&type=,1.10066664,3.72533321, 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, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248093&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248092&type=,1.10066664,3.72533321, and its internal standard ,15,NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248098&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248095&type=,1.10066664,3.72533321, were ,m,/,z, 46 and 47，while those for target NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248103&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248100&type=,1.10066664,3.72533321, and its internal standard ,15,NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248112&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248107&type=,1.10066664,3.72533321, were ,m,/,z, 62 and 63，respectively．There was a good linear relationship for NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248122&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248117&type=,1.10066664,3.72533321, in whole blood（,r,2, = 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, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248129&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248126&type=,1.10066664,3.72533321, in whole blood（,r,2, = 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, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248135&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248132&type=,1.10066664,3.72533321, and NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248142&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248139&type=,1.10066664,3.72533321, in 16 whole blood samples of healthy person were determined by this method．The results showed that the concentrations of NO, $2 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248151&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248145&type=,1.10066664,3.72533321, and NO, $3 -$ ,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248160&type=,http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=37248157&type=,1.10066664,3.72533321, 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．

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

Keywords

nitritenitratewhole bloodgas chromatography－negative chemical ionization－mass spectrometry（GC－NCI－MS）toxicological analysis

references

Xu Y，Wang Z，Sun Y J，Tian W，Feng D J，Zhou L L．China Meas. Test（许洋，王智，孙羽婕，田伟，冯德建，周黎黎．中国测试），2021，47（12）：58－63.

Su X K，Liu X F，Li Y X，Huang J J，Tan W Y，Tan X L，Yao L H．J. Prev. Appl. Med. 苏小可，刘晓峰，李映霞，黄瑾景，谭文艳，谭晓罗，姚令辉．应用预防医学），2019，25（4）：309－310，312.

Zhang H B．Med. Forum. （张华斌．基层医学论坛），2020，24（14）：2033－2034.

Tang J Q，Ye G H，Fan Y Y，Yu L S，Xu C Q，Hu H Y．Chin. J. Forensic Med. （汤家全，叶光华，范琰琰，喻林升，徐彩裙，胡海燕．中国法医学杂志），2014，29（3）：280.

Yi Z Y，Zuo X C，Peng G Z，Zhou H．Chin. J. Pub. Health Manage. 易智勇，左笑丛，彭广泽，周华．中国公共卫生管理），2006，（6）：524－527.

Kong W G，Zhang Z G，Yang X．Chin. J. Forensic Med. （孔维刚，张志国，杨旭．中国法医学杂志），2012，27（5）：417.

Li H Y，Zhang X L，Li X C．J. Instrum. Anal. （李海燕，张校亮，李晓春．分析测试学报），2016，35（11）：1403－1408.

Giustarini D，Rossi R，Milzani A，Dalle－Donne I．Methods Enzymol.，2008，440：361－380.

Zhan S Y，Shao Q，Liu L，Fan X H．Biomed. Chromatogr.，2013，27（11）：1547－1553.

Tatarczak－Michalewska M，Flieger J，Kawka J，Plazinski W，Flieger W，Blicharska E，Majerek D．Molecules，2019，24（9）：1－15.

Yan H，Zhuo X Y，Shen B H，Xiang P，Shen M．J. Forensic Sci.，2016，61（1）：254－258.

Zeng X L，Ye M L，Chen Y X，Zhu Y．J. Instrum. Anal. （曾雪灵，叶明立，陈永欣，朱岩．分析测试学报），2016，25（3）：92－94.

Morcos E，Wiklund N P．Electrophoresis，2001，22（13）：2763－2768.

Tsikas D，Schwarz A，Stichtenoth D O．Anal. Chem.，2010，82（6）：2585－2587.

Yang X B，Bondonno C P，Indrawan A，Hodgson J M，Croft K D．Free Radical Bio. Med.，2013，56：1－8.

Hanff E，Lützow M，Kayacelebi A A，Finkel A，Maassen M，Yanchev G R，Haghikia A，Bavendiek U，Buck A，Lücke T，Maassen N，Tsikas D．J. Chromatogr. B，2017，1047：207－214.

Ata S，Akyüz M，Dinc E．Int. J. Environ. Anal. Chem.，2016，96（7）：636－652.

Tsikas D．Free Radic. Res.，2005，39（8）：797－815.

Pagliano E，Campanella B，D'Ulivo A，Mester Z．Anal. Chim. Acta，2018，1025：12－40.

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