论文部分内容阅读
建立了1个基于Orbitrap技术的液质联用方法,对皮革及其制品中残留的20种有害有机溶剂进行了快速筛查和确证。皮革及其制品中残留的有害有机溶剂经超声提取后,所得萃取液经Waters Sep-Pak Vac Silica固相萃取柱(1 g/6 m L)净化,再进行超高效液相色谱/静电场轨道阱高分辨质谱分析,根据提取离子色谱峰面积进行外标法定量。20种有害有机溶剂在Hypersil GOLD色谱柱(100 mm×2.1 mm,1.9μm)上进行色谱分离,以甲醇/水为流动相,进行梯度洗脱。质谱分析采用电喷雾正离子(ESI+)模式,一级质谱全扫描范围为m/z 50~m/z 300,根据保留时间和准分子离子的精确质量数进行定性,根据二级质谱进行确证。该方法的定量限为0.5~10.0μg/kg,在3个不同加标浓度水平下平均加标回收率为81.7%~95.3%,相对标准偏差RSD为3.6%~11.5%。该方法灵敏度高,定性可靠,定量准确,可完全满足欧盟REACH法规的限量要求,并成功地应用于市售皮革及其制品中残留有害有机溶剂的快速筛查和确证。
An Orbitrap-based liquid chromatography-mass spectrometry (LC-MS / MS) method was established for the rapid screening and confirmation of 20 hazardous organic solvents remaining in leather and its products. After ultrasonic extraction of the harmful organic solvents remaining in the leather and its products, the resulting extract was purified with a Waters Sep-Pak Vac Silica SPE (1 g / 6 mL) and subjected to ultra performance liquid chromatography / electrostatic field orbit Well high-resolution mass spectrometry, according to the extracted ion chromatographic peak area for external standard quantitative. Twenty kinds of hazardous organic solvents were separated on a Hypersil GOLD column (100 mm × 2.1 mm, 1.9 μm) and eluted with a gradient of methanol / water. Mass spectrometry was performed using electrospray positive ion (ESI +) mode. The first full-scale MS range was m / z 50 ~ m / z 300. Qualitative analysis was based on the retention time and the exact mass of quasi- The limit of quantification was 0.5-10.0 μg / kg. The average recoveries were 81.7% -95.3% at 3 spiked levels and the relative standard deviations (RSDs) ranged from 3.6% to 11.5%. The method is highly sensitive, qualitative and reliable, quantitative and accurate, and can fully meet the REACH requirements of the EU. It has been successfully applied to the rapid screening and confirmation of residual harmful organic solvents in commercial leather and its products.