摘要
为快速、准确测定烟用包装材料中的高氯酸根,建立了测定烟用纸张(接装纸、内衬纸、条与盒包装纸)中高氯酸根离子的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经水提取、多级固相萃取柱净化后,采用阴离子分析柱,以乙腈-乙酸铵水溶液为流动相进行色谱分离,在多反应监测(MRM)模式下进行质谱测定。结果表明:1^(18)O标记高氯酸根离子内标的加入及样品的多级净化有效降低了基质效应;2在0.2~20.0μg/L质量浓度范围内,标准曲线线性关系良好(R2>0.995);加标回收率为95.2%~105.5%;日内和日间相对标准偏差均<8%;检出限和定量限分别为1.13和3.77μg/kg。3在所测定的100个样品中,高氯酸根离子的检出率为9%,最高检出量为0.048 mg/kg,远小于美国食品药品监督管理局(US FDA)所规定的食品包装材料中允许的最高限量。该方法操作简便、灵敏度高、准确性好,适用于烟用纸张中高氯酸根离子的测定。
In order to determine the perchlorate levels in cigarette packaging materials rapidly and accurately, a high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method was developed to quantify the perchlorate in papers used for cigarette （including tipping paper, inner liner paper, carton and packet packaging paper）. After extraction by water and multistep purified by SPE cartridges, the samples were separated on IC-Pak HR column with CH3CN-CH3CO2NH4 solution as mobile phase, and determined by mass spectrum under multiple reaction monitoring （MRM） mode. The results showed that： 1） With the multistep cleanup and addition of 180-labeled internal standard, the ion suppression at different concentrations was substantially alleviated. 2） The calibration curve was linear in the range of 0.2-20.0 μg/L with correlation coefficient more than 0.995. The mean values of intra- and inter-day RSDs were all less than 8%, the spiked recoveries ranged from 95.2% to 105.5%, and the LOD and LOQ were 1.13 and 3.77 μg/kg, respectively. 3） Using 100 tested samples, the detection rate of perchlorate was 9% with the highest level of 0.048 mg/kg, which was much lower than the maximum values regulated by US FDA. This method is convenient, sensitive, accurate and suitable for determination of perchlorate in papers for cigarette.
出处
《烟草科技》
EI
CAS
CSCD
北大核心
2016年第12期54-59,共6页
Tobacco Science & Technology
基金
中国烟草总公司标准项目"烟用材料部分物质(成分)检测方法研究(二期)"(512013AB0050)
