利用差示扫描量热单峰法开展了二苯并(b,f)-1,4-氧氮吖庚因的纯度分析。通过优化升温速率和样品质量,获得了最佳实验条件为:升温速率1.0℃/min,样品质量2.50～3.50mg。测得的二苯并(b,f)-1,4-氧氮吖庚因纯度平均值为99.35%,相对标准偏差(RSD)为0.033%(n=5)。与高效液相色谱(HPLC)法和核磁共振氢谱(1H-NMR)法的测试结果进行比较,相差不大。差示扫描量热单峰法简单、快速,准确度高,可作为二苯并(b,f)-1,4-氧氮吖庚因生产过程中产品的质量控制方法。
The purity of Dibenz(b,f)-1,4-oxaxepin was analyzed by monopeak method at differential scanning calorimetry.By optimizing the heating rate and the sample quality,the best experimental conditions were obtained:the heating rate was 1.0℃/min,and the sample quality was 2.5～3.5mg.The measured Dibenz(b,f)-1,4-oxaxepin purity was 99.35%,and the RSD was 0.033%(n=5).Compared with the test results of high performance liquid chromatography and nuclear magnetic resonance,there was not much difference.The monopeak method of differential scanning calorimetry was simple,fast and highly accurate,and can be used as a quality control method for products in the Dibenz(b,f)-1,4-oxaxepin production process.
[1] Olajos Eugene J,Salem Harry.Riot control agents:pharmacology,toxicology,biochemistry and chemistry[J].Journal of Applied Toxicology,2001,21(5):355-391.
[2] 林汉杰,姜滇.二苯并(b,f)-1,4-氧氮吖庚因在银胶体系中产生SERS的机理探讨[J].分析测试学报,1997,16(5):48-50.
[3] Rothenberg Craig,Achanta Satyanarayana,Svendsen Erik R,et al.Tear gas:an epidemiological and mechanistic reassessment[J].Annals of the New York Academy of Sciences,2016,1378(1):96-107.
[4] 左明,刘昌财.HPLC-ESI-MS/MS法测定二苯并(b,f)-1,4-氧氮吖庚因的氧化产物[J].应用化学,2008,25(11):1378-1380.
[5] Schep L J,Slaughter R J,McBride D I.Roit control agents:the tear gases CN,CS and OC--a medical review[J].Journal of the Royal Army Medical Corps,2015,161(2):94-99.
[6] 汪海涛,刘海峰,刘艳,等.多种分析方法测定氯代苯亚甲基丙二腈的纯度[J].应用化学,2020,37(7):810-815.
[7] Riches J R,Read R W,Black R M,et al.The development of an analytical method for urinary metabolites of the riot control agent 2-chlorobenzylidene malononitrile(CS)[J].Journal of Chromatography B,2013,928(1):125-130.
[8] Recer G M,Johnson T B,Gleason A K,et al.An evaluation of the relative potential public health concern for the self-defense spray active ingredients oleoresin capisucum,o-chlorobenzylidence malononitrile,and 2-chloroacetophenone[J].Regulatory Toxicology and Pharmacology,2002,36(1):1-11.
[9] Bag B C,Kaushik M P.Process monitoring of dibenz-[b,f]-1,4-oxazepine(CR) by gas chromatographic method[J].Indian Journal of Chemical Technology,2002,9(5):415-419.
[10] D’Agostino P A,Provost L R.Analysis of irritants by capillary column gas chromatography-tandem mass spectrometry[J].Journal of Chromatography A.1995,695(1):65-73.
[11] 陈栋华,李丽清,马治军.822e型DSC测定纯度的影响因素[J].中南民族大学学报(自然科学版),2002,21(1):4-7.
[12] 肖珍芳,李浩锋,罗建明,等.差示扫描量热仪的原理与应用[J].中国石油和化工标准与质量.2018,38(19):131-132.
[13] 陈咏萱,周东山,胡文兵.示差扫描量热法进展及其在高分子表征中的应用[J].高分子学报,2021,52(4):1-19.
[14] 丁恩勇,梁学海.对DSC单峰纯度测定法的评述[J].分析测试学报,1993,12(4):52-55.
[15] 李伟,丁宵霖,戴庆平,等.差示扫描量热法测定番茄红素的纯度[J].食品科学,2002,23(9):87-89.
[16] 段晶钟,汪海涛,刘海峰,等.差示扫描量热单峰法测定苯氯乙酮的纯度[J].化学分析计量,2020,29(5):8-18.
[17] 陈青,魏伯荣,包德君.差示扫描量热法单峰测定物质的纯度[J].分析仪器,2005(3):42-46.
[18] 常伟伟,彭辉.差示扫描量热法测定对乙酰氨基酚原料药纯度[J].化学分析计量,2020,29(2):36-39.
[19] 王昉,涂强,李意,等.差示扫描量热分析法测定米力农药物的纯度[J].化学世界,2012,53(6):338-341.
[20] 王娟,张顺,林萍,等.差示扫描量热法测定衣康酸纯度和熔点[J].高科技纤维与应用,2018,43(4):21-24.
[21] 徐冬梅,韩晓强,张焱,等.差示扫描量热法测定柠檬酸纯度[J].新疆石油科技,2005,15(2):38-40.
[22] 王萌玉,金灿,孙永跃,等.氢定量核磁共振法测定金丝桃苷标准物质纯度[J].化学试剂,2020,42(4):425-429.
[23] Xue Tian,Cui Qingzhong,Han Yonghe.Hyphenated techniques of thermal analysis for dibenz[b,f][1,4] oxazepine[J].Analytical Methods,2016(8):3824.
