Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction
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摘要: 近年人工合成麝香在环境中污染状况加剧，该类化合物具有潜在致癌和环境激素作用，对人类健康构成了威胁，因此越来越受到科学工作者的重视。水和土壤等环境样品中的人工合成麝香检测技术发展迅速，并朝着快速绿色的方向发展。人工合成麝香在沉积物中的浓度达到了几个到几千个ng/g的水平，但对于沉积物复杂基质中的多种类人工合成麝香，采取同步提取与净化，并快速分析的方法还有待研究。本文建立了沉积物样品中硝基麝香、多环麝香和大环麝香共三类、14种典型人工合成麝香的快速分析方法。通过实验优化了提取溶剂、提取温度、在线净化吸附剂等条件，大大降低了样品的前处理成本。最终确定样品采用加速溶剂萃取，萃取池中依次装入净化吸附剂（0.4g GCB和1.0g SAX）及5.0g沉积物样品，在80℃条件下采用提取溶剂正己烷-丙酮（4：1，V/V）循环提取2次，提取液浓缩后采用气相色谱-三重四极杆串联质谱（GC-MS/MS）进行测定。结果表明：14种目标化合物的线性范围为5~200ng/mL，平均添加回收率为70.6%~121.5%，相对标准偏差（RSD，n=7）为0.97%~19.5%。替代物回收率为72.2%~116.8%，方法检出限为硝基麝香0.10~0.19ng/g，多环麝香0.09~0.14ng/g，大环麝香0.11~1.93ng/g。该方法能够满足复杂基质沉积物样品的分析要求。
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关键词:
- 人工合成麝香 /
- 沉积物 /
- 气相色谱-三重四极杆串联质谱法 /
- 加速溶剂萃取 /
- 复杂基质样品
Abstract:BACKGROUNDIn recent years, the pollution of synthetic musk in the environment has increased. This kind of material has potential carcinogenic and environmental hormone effects and poses a threat to human health. Therefore, it has attracted increasing attention from scientists. The analytical technology of synthetic musk in environmental samples such as water and soil has developed rapidly. The concentration of synthetic musk in sediments has reached several thousand ng/g, but the methods for the simultaneous extraction and purification and rapid analysis of various types of synthetic musk in complex matrices of sediments are yet to be studied. OBJECTIVESTo establish a rapid method for the analysis of 14 typical synthetic musks in sediment samples by accelerated solvent extraction (ASE) combined with gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). METHODSAccelerated solvent extraction was used for sample preparation. The ASE cell was filled up with sorbent (0.4g GCB combined with 1.0g SAX) and 5.0g sediment samples. The sample was extracted in two cycles with mixed solvents hexane-acetone (V/V, 4:1) at 80℃. After preconcentration, the extracted solution was determined by GC-MS/MS. RESULTSThe linear range of this method for fourteen target compounds ranged from 5ng/mL to 200ng/mL. The average spike-added recoveries ranged from 70.6% to 121.5%, the relative standard deviations (RSD, n=7) were 0.97%-19.5%. The recoveries of surrogates were 72.2%-116.8%. The detection limits of the method were 0.10-0.19ng/g for nitro musk, 0.09-0.14ng/g for polycyclic musk, and 0.11-1.93ng/g for macrocyclic musk. CONCLUSIONSThis method can satisfy the analysis of musk in sediments with complex matrices. -
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表 1 目标化合物的保留时间、监测离子对和碰撞能量
Table 1. Retention times, monitoring ion pairs and collision energies of target compounds
化合物 保留时间(min) 离子对(m/z) 碰撞能量(eV) 开司米酮 8.767 191>135▲
191>163126 萨利麝香 12.830 229>173▲
229>57918 粉檀麝香 13.670 229>187▲
229>57615 菲-d10 14.450 188>160▲
188>1582130 葵子麝香 15.155 268>253▲
253>79927 二甲苯麝香-d15 15.394 294>126▲
294>114633 特拉斯麝香 15.535 215>173▲
215>17196 佳乐麝香 15.646 243>213▲
243>1711518 二甲苯麝香 15.711 282>106▲
282>159219 3-甲基环十五烷酮 15.755 96>81▲
96>67912 吐纳麝香-d3 15.757 246>190▲
246>57921 吐纳麝香 15.801 243>187▲
243>57621 伞花麝香 16.215 263>221▲
263>128630 西藏麝香 17.001 251>147▲
251>117927 黄葵内酯 17.159 96>81▲
96>67612 麝香酮 17.604 279>118▲
279>191249 麝香T 18.190 227>55▲
227>163246 注：“▲”表示定量离子对。 
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表 2 净化吸附剂对目标物提取回收率的影响
Table 2. Effect of different purification adsorbents on extraction recovery of target compounds
化合物 目标物回收率(%) 1.0g SCX 1.0g SAX 0.5g GCB 0.5g炭黑 0.2g GCB+1.0g SAX 0.4g GCB+1.0g SAX 0.5g GCB+1.0g SAX 开司米酮 120.3 86.3 85.6 87.5 83.7 103.5 101.9 萨利麝香 128.1 93.5 91.9 106.8 104.4 95.6 96.6 粉檀麝香 126.9 94.9 92.9 114.8 104.9 96.2 97.4 葵子麝香 97.6 99.1 96.4 129.5 112.3 97.5 97.8 二甲苯麝香-d15 106.3 81.7 81.9 84.1 98.1 104.6 103.2 特拉斯麝香 171.0 97.6 99.1 107.0 112.7 96.8 97.2 佳乐麝香 - 98.2 100.3 106.6 114.9 99.7 100.6 二甲苯麝香 120.7 96.4 89.2 63.3 99.8 93.1 94.8 3-甲基环十五烷酮 - 111.3 131.4 93.7 126.8 86.6 83.7 吐纳麝香-d3 203.8 88.1 92.5 138.1 102.1 104.3 105.5 吐纳麝香 3168.1 88.8 92.4 100.3 97.4 97.3 98.1 伞花麝香 109.9 103.4 104.0 67.5 94.6 103.7 103.9 西藏麝香 127.8 101.5 110.9 91.9 103.8 94.1 93.5 黄葵内酯 - 127.9 123.8 1000.2 113.9 81.4 86.2 麝香酮 224.4 116.6 108.6 82.4 125.3 95.8 95.9 麝香T - 109.1 107.8 115.9 123.0 99.4 101.7 注：“-”表示未检出，下表同。
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表 3 目标物测定线性范围、相关系数、相对标准偏差、平均回收率及方法检出限
Table 3. Linear range, correlation coefficients, relative standard deviation (RSD), average recovery and detection limit of the method for target compounds
化合物 线性范围(ng/mL) 相关系数(R2) 平均回收率(%)及相对标准偏差(%，n=7) 方法检出限(ng/g) 0.5ng/g 5.0ng/g 10.0ng/g 开司米酮 2~200 0.9977 121.5 4.80 101.1 2.94 70.6 2.34 0.09 萨利麝香 2~200 0.9980 98.5 8.56 92.7 2.16 85.3 0.97 0.13 粉檀麝香 2~200 0.9980 97.1 8.89 93.6 1.81 84.7 1.31 0.14 葵子麝香 2~200 0.9960 86.2 11.8 95.6 5.08 85.7 4.50 0.16 特拉斯麝香 2~200 0.9981 97.8 8.20 93.9 1.78 90.7 3.29 0.13 佳乐麝香 2~200 0.9981 118.3 5.00 97.2 2.86 84.8 2.36 0.09 二甲苯麝香 2~200 0.9983 94.4 12.6 88.9 6.92 84.0 3.02 0.19 3-甲基环十五烷酮▲ 10~200 0.9978 84.4 14.6 109.6 8.55 88.2 10.9 1.93 吐纳麝香 2~200 0.9982 97.9 6.43 94.8 1.43 80.8 3.64 0.10 伞花麝香 2~200 0.9959 101.2 8.01 101.2 5.00 90.0 5.03 0.13 西藏麝香 2~200 0.9975 91.4 9.00 91.0 3.10 87.8 3.29 0.13 黄葵内酯 2~200 0.9986 95.8 11.8 80.3 5.52 109.4 6.33 0.18 麝香酮 2~200 0.9974 84.8 7.23 94.3 3.18 116.5 5.09 0.10 麝香T 2~200 0.9984 94.0 7.50 97.2 1.98 96.1 4.97 0.11 二甲苯麝香-d15 - - 92.9 9.47 94.6 6.05 81.5 19.5 - 吐纳麝香-d3 - - 106.1 2.62 100.9 1.40 82.7 9.65 - 注：“▲”表示添加水平为5.0、10.0、20.0ng/g。
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表 4 各类样品目标物分析方法检出限的比较
Table 4. Comparison of detection limit of the method for target compounds in different samples
样品类型 待测物数量(个) 分析方法 方法检出限(ng/g) 参考文献 多环麝香 硝基麝香 大环麝香 土壤 5 2 - SE-GC-MS 0.03~0.33 [18] 土壤、底泥 2 - - MAE-GC-MS 0.66~0.72 [19] 污泥、底泥、土壤 5 2 - ASE-GC-MS 0.25~0.33 [20] 土壤 2 - - ASE-GC-MS 0.19和0.295 [21] 污泥 - - 8 SPME-GC-MS 0.010~0.025 [25] 污泥、沉积物 6 - - SPME-GC-MS 0.04~0.1 [26] 污泥 5 4 - SPME-GC-MS 0.049~0.611 [27] 土壤 6 2 - SBSE-TD-GC-MS 0.01~1.1 [28] 污泥 6 3 4 SBSE-TD-GC-MS 5~30 [29] 沉积物 6 5 3 ASE-GC-MS/MS 0.09~0.19和1.93 本方法
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表 5 实际沉积物样品中人工合成麝香检测结果
Table 5. Analytical results of synthetic musks in real sediment samples
样品序号 含量(ng/g) 佳乐麝香(HHCB) 吐纳麝香(AHTN) 1 0.17 0.11 2 0.17 - 3 0.09 - 4 0.40 0.20 5 - - 6 0.36 0.16 7 0.21 - 8 0.09 - 9 0.09 - 10 0.21 - 11 - - 12 0.18 - 13 0.12 - 14 - - 15 - - 16 0.10 - 17 0.09 - 18 0.19 - 19 - - 20 0.12 -
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