[1]彭睿,马越,张文艺.顶空固相微萃取/气质联用测定水中10种致嗅物质[J].中国给水排水,2023,39(18):147-154.
　PENGRui,MAYue,ZHANGWen-yi.Online Headspace Solid-phase Microextraction/Gas Chromatography-Mass Spectrometry for Determination of Ten Odorous Compounds in Water[J].China Water & Wastewater,2023,39(18):147-154.
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顶空固相微萃取/气质联用测定水中10种致嗅物质

中国给水排水[ISSN:1000-4062/CN:12-1073/TU] 卷: 第39卷 期数: 2023年第18期 页码: 147-154 栏目: 出版日期: 2023-09-17
Title:
Online Headspace Solid-phase Microextraction/Gas Chromatography-Mass Spectrometry for Determination of Ten Odorous Compounds in Water
作者:
彭睿， 马越， 张文艺
（深圳市深水龙华水务有限公司，广东 深圳 518110）
Author(s):
PENG　Rui， MA　Yue， ZHANG　Wen-yi
（Shenzhen Shenshui Longhua Water Co. Ltd.， Shenzhen 518110， China）
关键词:
致嗅物质;  固相微萃取;  气相色谱-质谱法
Keywords:
odorous compounds;  solid-phase microextraction;  GC-MS
摘要:
采用顶空固相微萃取/气相色谱质谱法测定水体中二乙基二硫醚、二甲基三硫醚、2，4-辛二烯醛、正壬醇、2-异丙基-3-甲氧基吡嗪、β-环柠檬醛、吲哚、2，4，6-三氯苯甲醚、2-甲基异莰醇、土臭素等10种微生物源致嗅物质。用单因素实验优化了气相色谱升温程序、固相微萃取纤维头涂层、氯化钠加入量、萃取温度、萃取时间、解吸时间。结果表明，使用85 μm CAR/PDMS 萃取纤维头、每10 mL水样中加入3.5 g氯化钠、于80 ℃萃取温度下萃取60 min、于250 ℃进样口中解吸5 min时，对10种嗅味物质的测定效果良好。同时，在《生活饮用水标准检验方法 第8部分：有机物指标》（GB/T 5750.8—2023）推荐的2-甲基异莰醇检测方法基础上，将2-甲基异莰醇与内标物2-异丁基-3-甲氧基吡嗪保留时间附近处的升温速率调整至0 ℃/min，可有效避免两物质难以分离，从而导致低浓度下2-异丁基-3-甲氧基吡嗪在95 m/z处的碎片会影响2-甲基异莰醇定量的问题。在此条件下，10种嗅味物质在5.0~80.0 ng/L范围内线性良好，方法检出限为0.05~3.26 ng/L，加标回收率为74.3%～128.1%，相对标准偏差为1.9%～14.4%。此方法预处理简便、检测快速、灵敏度高，适用于水体中10种微生物源致嗅物质的检测。
Abstract:
A headspace solid-phase microextraction/gas chromatography-mass spectrometry method was used to determine 10 microbial-derived odorous compounds in water, including diethyl disulfide, dimethyl trisulfide, 2,4-octadiene aldehyde, n-nonanol, 2-isopropyl-3-methoxypyrazine, β-cyclocitral, indole, 2,4,6-trichloroanisole, 2-methylisoborneol and geosmin. The gas chromatography ramp-up procedure, solid phase microextraction fiber head coating, dosage of sodium chloride, extraction temperature, extraction time and desorption time were optimized by single factor experiments. The 10 microbial-derived odorous compounds were well detected under the following conditions: 85 μm CAR/PDMS extraction fiber head, adding 3.5 g of sodium chloride to every 10 mL of water sample, extracting at 80 ℃ for 60 min and desorption at 250 ℃ for 5 min in the injection port. Based on the 2-methylisoborneol detection method recommended in Standard Examination Methods for Drinking Water—Part 8:Organic Indices, the temperature rise rate near the retention time of 2-methylisoborneol and 2-isobutyl-3-methoxypyrazine was adjusted to 0 ℃/min, which effectively avoided the 2-isobutyl-3-methoxy pyrazine fragments at 95 m/z at low concentration affecting the quantification of 2-methylisobornol caused by the difficult separation between 2-methylisoborneol and 2-isobutyl-3-methoxypyrazine. Under these conditions,the linearity of the 10 microbial-derived odorous compounds was good in the range of 5.0-80.0 ng/L, the detection limits were 0.05-3.26 ng/L, the spiked recoveries were between 74.3% and 128.1%, and the relative standard deviations were 1.9%-14.4%. This analytical method is simple, rapid and sensitive, and is suitable for the detection of 10 kinds of microbial-derived odorous compounds in water.
更新日期/Last Update: 2023-09-17