| 气相色谱-串联质谱法测定卷烟主流烟气中7种酚类化合物 |
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| 引用本文： | 吴永良,李燕垣,彭云铁.气相色谱-串联质谱法测定卷烟主流烟气中7种酚类化合物[J].质谱学报,2018,39(3):376-384. |
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| 作者姓名： | 吴永良 李燕垣 彭云铁 |
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| 作者单位： | 广东省质量监督烟草检验站，广东 广州510610 |
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| 摘 要： | 建立了气相色谱-串联质谱（GC-MS/MS）法检测卷烟主流烟气中苯酚、邻甲酚、间甲酚、对甲酚、邻苯二酚、间苯二酚、对苯二酚7种酚类化合物。在标准抽吸条件下，用剑桥滤片收集5支卷烟主流烟气粒相物，经异丙醇超声提取后，利用GC-MS/MS的多反应监测模式（MRM）测定，内标法定量。在优化的前处理及仪器条件下，7种酚类化合物呈现良好的线性关系（R2≥0.998 6），定量限为0.012~0.021 μg/cig，加标回收率为91.1%~107.7%，相对标准偏差（RSD）为2.5%~6.6%。该方法操作简单、分析时间短、准确可靠、灵敏度高，适用于卷烟主流烟气中酚类化合物的检测分析。
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| 关 键 词： | 卷烟 主流烟气 酚类 气相色谱-串联质谱（GC-MS/MS） |
Determination of Seven Phenolic Compounds in Mainstream Cigarette Smoke by Gas Chromatography-Tandem Mass Spectrometry |
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| WU Yong-liang,LI Yan-yuan,PENG Yun-tie.Determination of Seven Phenolic Compounds in Mainstream Cigarette Smoke by Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Chinese Mass Spectrometry Society,2018,39(3):376-384. |
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| Authors: | WU Yong-liang LI Yan-yuan PENG Yun-tie |
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| Affiliation: | Guangdong Tobacco Quality Supervision and Test Station, Guangzhou 510610, China |
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| Abstract: | A method for simultaneous determination of 7 phenolic compounds (phenol, o-cresol, m-cresol, p-cresol, catechol, resorcinol, hydroquinone) in mainstream cigarette smoke was developed using gas chromatography-tandem mass spectrometry (GC-MS/MS). The total particulate matter (TPM) of 5 cigarettes in mainstream cigarette was trapped by a 44 mm Cambridge filter pad with a Cerulean SM450 smoking machine under standard smoking condition. The filter pad which collected TPM was extracted on an ultrasonic generator for 20 min with 50 mL isopropanol and 100 μL ISTD solution containing 1 mg/L of 1-phenylethyl propionate. The solution extract was filtered through 0.45 μm pore size nylon filters, and then was analyzed by GC-MS/MS under multiple reaction monitoring (MRM) mode and was determined by ISTD method under the optimized conditions. In order to get good extraction efficiencies of phenolic compounds during a short time, 4 different extraction solvents (cyclohexane, dichloromethane, isopropanol, methanol) , 3 different extraction solvent volumes (20, 50, 100 mL) and 6 different ultrasonic extraction times (5, 10, 20, 30, 40, 60 min) were tested. The optimum condition was that 50 mL isopropanol extracted for 20 min. 4 compounds (propyl benzoate, 1-phenylethyl propionate, n-heptadecane, benzyl benzoate) were tested for choosing the suitable ISTD compounds. The results indicate that propyl benzoate and 1-phenylethyl propionate are suitable for ISTD compounds. 3 different polarity capillary columns (HP-5MS UI, DB-35MS, HP-INNOWAX) with the same column dimensions (30 m×0.25 mm×0.25 μm) were inspected. Both the best separation and peak shapes of seven phenolic compounds are achieved on the HP-5MS UI capillary column. The results showed that the linearity of phenols were above 0.998 6. The limits of quantification (LOQs) were 0.012-0.021 μg/cig. The recoveries were 91.1%-107.7% with the relative standard deviations (RSDs) lower than 6.6%. It was clearly advantageous for assays of phenolic compounds present in complicated matrices of mainstream cigarette smoke. As a part of the validation procedure, 12 brands of cigarettes were tested by the designed method. This method is suitable for the rapid determination of seven phenolic compounds in mainstream cigarette smoke with easy operation, high sensitivity, excellent precision and high throughput. |
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| Keywords: | cigarette mainstream smoke phenolic compounds (phenols) gas chromatography-tandem mass spectrometry (GC-MS/MS) |
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