摘要
目的建立工作场所空气中N-甲基-2-吡咯烷酮(NMP)的溶剂解吸气相色谱测定方法。方法工作场所空气中NMP用活性炭管采集,经甲醇︰二氯甲烷(5∶95,V/V)解吸后,毛细管色谱柱分离,火焰离子化检测器测定。结果 NMP质量浓度在0.51~4 108.00 mg/L时线性关系良好,相关系数为0.999 9,检出限为0.08 mg/L(以3倍标准差计算)。方法平均解吸效率为101.68%~103.44%,批间、批内相对标准偏差分别为1.94%~3.97%、0.97%~2.26%。样品在室温下可保存14 d。结论本方法适用于工作场所空气中NMP的采样与检测。
Objective To establish a method for determination of N-methyl-2-pyrrolidone(NMP) in workplace air by solvent desorption-gas chromatography. Methods NMP in the workplace air was collected with activated carbon tube and desorbed with methanol ∶dichloromethane(5 ∶95, V/V). After desorption, it was separated by capillary column separation, and detected by flame ionization detector. Results The good linear concentration of NMP was 0.51-4 108.00 mg/L. The correlation coefficient was 0.999 9. The detection limit was 0.08 mg/L(calculated by 3 times of standard deviation). The average desorption efficiency was 101.68%-103.44%. The within-run and between-run relative standard deviations were 1.94%-3.97% and 0.97%-2.26%, respectively. The sample could be stored at room temperature for at least 14 days. Conclusion The developed method is suitable for the determination of NMP in workplace air.
引文
[1] 欧玉静,王晓梅,李春雷,等.N-甲基吡咯烷酮的应用进展[J].化工新型材料,2017,45(8):270-272.
[2] 刘美,刘金东,盖钰垚,等.N-甲基吡咯烷酮(NMP)在石油化工中的应用进展[J].应用化工,2017,46(5):991-994.
[3] SITAREK K,STETKIEWICZ J.Assessment of reproductive toxicity and gonadotoxic potential of N-methyl-2-pyrrolidone in male rats[J].Int J Occup Med Environ Health,2008,21(1):73-80.
[4] SITAREK K,KILANOWICZ A.Tissue distribution and excretion of N-methyl-2-pyrrolidone in male and female rats[J].Int J Occup Med Environ Health,2006,19(2):142-148.
[5] JUNGBAUER F H W,COENRAADS P J,KARDAUN S H.Toxic hygroscopic contact reaction to N-methyl-2-pyrrolidone[J].Contact Dermatitis,2010,45(5):303-304.
[6] The National Institute for Occupational Safety and Health.ICSC#0513.2014[EB/OL].(2015-07-22)[2019-03-21].https://www.cdc.gov/niosh/ipcsneng/neng0513.htmL
[7] 古小明,钟学飘,刘双喜,等.1起急性N-甲基吡咯烷酮中毒的调查[J].中国职业医学,2010,37(4):358-359.
[8] 中华人民共和国卫生部.职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法:GBZ/T 210.4—2008[S].北京:人民卫生出版社,2008.
[9] 中华人民共和国卫生部.工作场所空气中有害物质监测的采样规范:GBZ 159—2004[S].北京:人民卫生出版社,2006.
[10] 柯宗枝,郑丽辉,万玲利,等.气相色谱测定法测定工作场所空气中N-甲基吡咯烷酮[J].中国卫生检验杂志,2017,27(17):2433-2435.
[11] 廖惠云,王珂清,庄亚东,等.气相色谱-质谱联用内标法测定干性食品包装纸中的N-甲基吡咯烷酮[J].包装工程,2013,34(21):6-11.
[12] 李天宝,王春利,刘炜,等.固相萃取-气相色谱-质谱法测定N-甲基吡咯烷酮[J].工业水处理,2014,34(3):75-77.
[13] The National Institute for Occupational Safety and Health.Manual of Analytical Methods(NMAM).N-methyl-2-pyrrolidone:Method1302,Issue 1[EB/OL].(1998-01-15)[2019-03-21].https://www.cdc.gov/niosh/docs/2003-154/pdfs/1302.pdf.
[14] 张福浩,武志燕,刘颖,等.N-甲基吡咯烷酮与乙醇溶液介电常数的特异性研究[J].化学研究与应用,2016,28(5):724-726.
[15] SCIALLI A R.The challenge of reproductive and developmental toxi-cology under REACH[J].Regul Toxicol Pharmacol,2008,51(2):244-250.