A method of determination of the migration of bisphenol A from plastic nursing bottle by GC was established.Used water as a leaching solution and then this liquid was extracted by solid phase extraction (SPE).After derivatization with perfluoropropionic anhydride (PFPA),the derivatives were determined by GC-ECD.The limit of detection was 0.2μg/L,the linear ranges were from 0.2 to 50μg/L with correlation coefficients of 0.9994.The average recoveries were in the range of 92.3%～98.5% with three different spiked levels,and the relative standard deviations ranged from 3.35%～5.96%(n=3).The method was sensitive,accurate,repeatable,and could be applied for the determination of the migration of small quantities of bisphenol A from plastic nursing bottle.

A confirmatory method was developed for the determination of polycyclic aromatic hydrocarbons in Material of Electronic products by GC-MS.Samples were extracted by using a solvent mixture of acetone and n-hexane(1+1) in Soxlet's Extraction and Purified with the silica gel column by washing a solvent mixture of n-hexane and dichloromethane(3+2).The detection limits of method were 0.2mg/kg.The average recoveries were in the range of 59%～99%,and the relative standard deviations(RSDs) were less than 5%.The standard curves for polycyclic aromatic hydrocarbons was in the range of 0.1mg/L～ 100mg/L.The method was simple,credible,and meet the test requirement of polycyclic aromatic hydrocarbons in electronic products.

建立了采用自动索氏萃取-气相色谱-质谱联用检测电子电气产品中多环芳烃和多氯联苯的方法。通过以V(丙酮)∶V(正己烷)=1∶1为溶剂,一次自动索氏提取材料中多环芳烃和多氯联苯,分别采用H2SO4预处理,再用硅胶柱净化,气相色谱-质谱联用仪检测,该方法对多环芳烃检测限为0.2 mg/kg、多氯联苯检测限为0.1 mg/kg,加标回收率在60%～99%之间,相对标准偏差(RSD)均小于5%,多环芳烃的线性范围在0.1～100 mg/L,多氯联苯的线性范围在0.4～250 mg/L,相关系数(r)均大于0.999。实验结果表明方法能满足电子电气产品材料中多环芳烃和多氯联苯的检测要求。

A confirmatory method is presented for the determination of polychlorinated biphenyls in Material of Electronic products by Soxlet's Extraction-GC-MS.Samples are extracted using a solvent mixture of acetone and n-hexane(1+1),Purified with the silica gel column.The detection limits of method were 0.1mg/kg,the recoveries were in the range of 60%～ 99%,and the relative standard deviations(RSDs) were less than 6%.The standard curves for polychlorinated biphenyls was linear in the concentration range of 0.4mg/L～250mg/L.It proved that the method was simple,credible,and meet the test requirement of polychlorinated biphenyls in Material in electronic products.

本研究采用加入甲醇与甲苯二异氰酸酯衍生反应的方式,避免了因水分、进样口温度等因素对检测甲苯二异氰酸酯的影响;同时,本方法应用程序升温,毛细管柱色谱分离,甲醇与甲苯二异氰酸酯衍生物测定可作为一种新的定性手段,确认油漆中未反应的甲苯二异氰酸酯(TDI)存在.建立了同时测定苯、甲苯、二甲苯和TDI异构体的定量测定方法.

美国公职分析化学家协会(AOAC)的"公定分析方法"969.09采用分光光度法测定农药百草枯中有效成分的含量.该方法是测定百草枯含量的经典和权威方法.虽然方法对一些操作条件做了较严格的规定,但显色反应产生的自由基仍然不稳定,方法不易操作,结果的准确性受到影响.本研究对操作和还原条件做了改进,明显提高了自由基的稳定性,并提出了优于原方法的优化条件.

[目的]建立了高效毛细管区带电泳技术同时快速测定饲料中的盐酸克伦特罗与沙丁胺醇的方法.[方法]采用单一有机试剂对饲料中的盐酸克伦特罗与沙丁胺醇进行提取,无需净化即可进行检测.通过对不同条件的考察,建立了前处理和电泳分析的最佳条件.[结果]方法对盐酸克伦特罗的添加回收率为7896-92%,最低检测限为0.5mg/kg:对沙丁胺醇的添加回收率为74%-87%,最低检出限为0.5mg/kg.[结论]这是一种适用于饲料中盐酸克伦特罗和沙丁胺醇同时检测的快速、准确、低成本方法.

A method for the separation and determination of terpineol oil by temperature programming capillary gas chromatography has been established. An OV-1 fused silica capillary column (30 m x 0.32 mm i.d. x 0.25 microns) was used with a temperature increase rates of 1.5 degrees C/min from 70 degrees C to 100 degrees C, 5 degrees C/min from 100 degrees C to 160 degrees C, 10 degrees C/min from 160 degrees C to 220 degrees C and then hold for 2 min. The main chemical components and their relative contents of the terpineol oil, terpinene oil, red and yellow oils of middle oils in the terpineol production and natural terpineol were analyzed by capillary gas chromatography-Fourier transform infrared spectrometry (GC-FTIR) and gas chromatography-mass spectrometry (GC-MS). The typical chromatograms of these oils are given. It has offered the information of the boiling points of the chemical compounds, and it is helpful to reutilize them after their separation by rectification. The results showed that the main compounds of the heavy cut of terpineol were longifolene and beta-caryophyllene. They are from the raw material, terpinene oil. The main compounds in the natural terpineol oil were eucalyptol, trans-4-thujanol, p-isopropenyl toluene, cis-4-thujanol, linalool, camphor, borneol, 4-terpineol, alpha-terpineol and safrole. The contents of beta-terpineol and gamma-terpineol were not so high as in synthetic terpineol.