CN112578070A - 一种测定海水中乙二醇含量的气相色谱-质谱检测方法 - Google Patents
一种测定海水中乙二醇含量的气相色谱-质谱检测方法 Download PDFInfo
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Abstract
本发明属于分析检测领域,涉及一种测定海水中乙二醇含量的气相色谱‑质谱检测方法,包括以下步骤:取适量样品于离心管中,加入氢氧化钠溶液,离心后取清液,再分别加入氢氧化钠溶液和苯甲酰氯试剂,震荡混匀,加入正己烷进行萃取,取正己烷层,供气相色谱‑质谱分析,保留时间和碎片离子定性,外标法定量。本方法简单快捷,定性定量准确,满足日常检测需要。
Description
技术领域
本发明属于分析检测领域,涉及一种测定海水中乙二醇含量的气相色谱-质谱检测方法。
背景技术
乙二醇(Ethylene Glycol,EG),CAS 107-21-1,又名甘醇、1,2-亚乙基二醇。分子式为C2H6O2,相对分子量为62.068,结构如式1所示。乙二醇是一种无色澄清粘稠液体,沸点198℃,闪点116℃,与水、低级脂肪族醇、甘油、醋酸、丙酮及类似酮类、醛类、吡啶及类似的煤焦油碱类混溶,在醚类中溶解度较小。
式1乙二醇结构式
乙二醇是一种重要的有机化工原料,用途十分广泛,主要用于生产PET纤维、防冻剂和精细化学品等。此外,乙二醇还可作为不饱和聚酯树脂、润滑剂、增塑剂、非离子表面活性剂以及炸药等原料,也常用作高沸点溶剂。由于乙二醇60%的水溶液的凝固点为-40℃,所以常被用作冬季汽车散热器的防冻剂和飞机发动机的制冷剂。
乙二醇具有一定的毒性,对人体的肾、肝、胃、肠道等内脏有损伤作用,可引发头晕、头痛、恶心、腹痛、口干、舌燥、出冷汗等症状。并且乙二醇在生产过程中容易产生大量含有乙二醇、二乙二醇和三乙二醇等污染物的工业废水。据国内外研究资料表明,处理乙二醇废水方法有电解法、湿式氧化法、臭氧法、反渗透法、化学氧化法、蒸馏法、生物法等。然而,虽然有些处理方法的效果较好,但由于处理费用高难以实现规模化,可能出现未完全处理的乙二醇废水外排现象,进而可能导致当地的河流乃至海洋环境遭受乙二醇污染,进而由点源向面源进行扩散。
自2017年起,各级海洋环境监管部门对我国管辖海域重点开展了海水质量、沉积物质量、生物多样性状况、入海河流污染物等项目的监测工作,除重点开展常规监测项目外,也会考量当地工业企业生产情况,因地制宜地开展特定污染物的监测工作,其中乙二醇成为部分地区的重点监测项目。
目前,我国并未制定水质中乙二醇的相关限量和检测标准。目前相关研究多为研究饮用水、废水、尿液等水基质乙二醇含量的测定方法,针对海水基质中乙二醇含量的测定方法的研究较少,其中,有使用固相萃取-气相色谱法检测海水中乙二醇的含量,该方法有较高的灵敏度、准确度和较低的检出限,但固相萃取的方法成本较高且耗时较长。本研究利用乙二醇在碱性条件下与苯甲酰氯反应产生苯甲酸乙二酯的原理(如式2所示),采用衍生的前处理方法有效提取海水基质中的乙二醇,考虑到海水中含有Ca2+、Mg2+等离子,加入碱性溶液后产生Ca(OH)2、Mg(OH)2等沉淀,干扰乙二醇与苯甲酰氯的反应,因此采用分段添加碱性溶液,有效去除Ca2+、Mg2+等离子对衍生反应的干扰,同时又能有效提取海水基质中的乙二醇,快速、准确测定海水中乙二醇含量,对海水中乙二醇含量的监测检测具有重要意义,为海水中乙二醇含量检测提供技术支撑。
式2衍生反应式
发明内容
本发明的目的是提供一种测定海水中乙二醇含量的气相色谱-质谱检测方法。
为了实现本发明的目的,本发明的技术方案如下:
(1)仪器条件
1)气相色谱条件
采用色谱柱DB-WAX ms(30mm×0.25mm×0.25μm),恒流,柱流量1.0mL/min;进样体积1.0μL;分流进样,分流比5∶1;进样口温度300℃;升温程序为初始温度185℃,保持3min,然后以20℃/min升至245℃,保持17min;
2)质谱条件
EI电离方式,电离能量70eV,离子源温度230℃,传输线温度300℃,溶剂延迟时间为3min,选择离子模式扫描,特征碎片离子定性定量;
(2)建立标准曲线
称取适量乙二醇标准物质,水溶解并定容,配制成1000.0mg/L的标准储备液,4℃密封储存;量取一定体积的标准储备液,经水稀释,配制成100.0mg/L的标准中间液,4℃密封储存;分别量取适量标准中间液,经水稀释,配制成0.01、0.10、0.50、1.00、2.00、5.00mg/L的系列标准工作液;分别量取5.0mL系列标准工作液,加入10mL蒸馏水,混匀,加入3.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;
依照“(1)仪器条件”分析上述滤液,以目标物定量离子的峰面积为纵坐标,以相应的浓度为横坐标绘制标准曲线;
(3)样品前处理
精确量取5.0mL水样于离心管中,加入1.0mL氢氧化钠溶液,漩涡混匀,5000r/min离心5min,取上清液;在沉淀中加入5mL蒸馏水,漩涡混匀,5000r/min离心5min,取上清液;重复清洗沉淀2次,合并上清液,漩涡混匀,5000r/min离心5min,取清液;
然后在上述清液中加入2.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;
(4)计算:外标法计算,按以下公式计算试样中目标物的含量:
X=c
上述公式中:
X——试样中待测物的含量,单位为毫克每升(mg/L);
c——样液浓度,单位为毫克每升(mg/L);
注:计算结果保留两位有效数字。
最优的,其定量离子为m/z 105,定性离子为m/z 51、77、270。
最优的,氢氧化钠溶液的浓度为40%(m/v),是将40.0g氢氧化钠溶于100mL水中,搅拌混匀后获得的。
最优的,该方法的检出限为0.01mg/L。
有益效果:本发明建立了一种测定海水中乙二醇含量的气相色谱-质谱检测方法。针对海水样品的特性,使用衍生方法,将海水中的乙二醇衍生为苯甲酸乙二酯,气相色谱-质谱分析,保证样品中的乙二醇能够完全参与反应,并且不受海水高盐的影响。本方法简单快捷,定量、定性准确,具有较高的回收率和精密度,能够满足海水样品的检测需求。
附图说明
结合附图和具体实施方式对本发明作进一步详细的说明:
图1乙二醇标准物质衍生产物总离子流色谱图
图2乙二醇标准物质衍生产物质谱碎片柱状图
图3标准曲线
图4海水阴性样品总离子流色谱图
图5海水阴性样品加标总离子流色谱图
具体实施方式
结合实施例对本发明做进一步说明,但不以任何方式对本发明加以限制,基于本发明所做出的任何变更或改进,均属于本发明的保护范围。
实施例一
称取适量乙二醇标准物质,水溶解并定容,配制成1000.0mg/L的标准储备液,4℃密封储存;量取一定体积的标准储备液,经水稀释,配制成100.0mg/L的标准中间液,4℃密封储存;量取适量标准中间液,经水稀释,配制成0.80mg/L的标准溶液;取5.0mL 0.80mg/L标准溶液,加入10mL蒸馏水,混匀,加入3.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;气相色谱条件:采用色谱柱DB-WAX ms(30mm×0.25mm×0.25μm),恒流,柱流量1.0mL/min;进样体积1.0μL;分流进样,分流比5∶1;进样口温度300℃;升温程序为初始温度185℃,保持3min,然后以20℃/min升至245℃,保持17min;EI电离方式,电离能量70eV,离子源温度230℃,传输线温度300℃,溶剂延迟时间为3min,选择离子模式扫描,监测碎片离子:m/z 105(定量离子)、51(定性离子)、77(定性离子)、270(定性离子)。其中,乙二醇标准物质衍生产物总离子流结果如图1,质谱碎片结果见图2。
实施例二
海水样品中乙二醇含量的测定
(1)标准曲线
分别量取实施例一中适量的标准中间液,经水稀释,配制成0.01、0.10、0.50、1.00、2.00、5.00mg/L的系列标准工作液;分别量取5.0mL系列标准工作液,加入10mL蒸馏水,混匀,加入3.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;标准曲线如图3所示;
(2)色谱条件
气相色谱条件:采用色谱柱DB-WAX ms(30mm×0.25mm×0.25μm),恒流,柱流量1.0mL/min;进样体积1.0μL;分流进样,分流比5∶1;进样口温度300℃;升温程序为初始温度185℃,保持3min,然后以20℃/min升至245℃,保持17min;
质谱条件:EI电离方式,电离能量70eV,离子源温度230℃,传输线温度300℃,溶剂延迟时间为3min,选择离子模式扫描,监测碎片离子:m/z 105(定量离子)、51(定性离子)、77(定性离子)、270(定性离子);
(3)样品测定
精确量取5.0mL水样于离心管中,加入1.0mL氢氧化钠溶液,漩涡混匀,5000r/min离心5min,取上清液;在沉淀中加入5mL蒸馏水,漩涡混匀,5000r/min离心5min,取上清液;重复清洗沉淀2次,合并上清液,漩涡混匀,5000r/min离心5min,取清液;然后在上述清液中加入2.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;
(4)定性定量结果
在保留时间窗口内未出现与目标物监测离子保留时间一致的色谱峰,说明样品未检出乙二醇,结果如图4所示。
实施例三
取实施例二中乙二醇检测结果为阴性的海水样品。
精确量取5.0mL水样于分液漏斗中,加入100.0mg/L的乙二醇标准中间液80μL,震荡混匀,静置30min。加入1.0mL氢氧化钠溶液,漩涡混匀,5000r/min离心5min,取上清液;在沉淀中加入5mL蒸馏水,漩涡混匀,5000r/min离心5min,取上清液;重复清洗沉淀2次,合并上清液,漩涡混匀,5000r/min离心5min,取清液;然后在上述清液中加入2.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;气相色谱条件:采用色谱柱DB-WAX ms(30mm×0.25mm×0.25μm),恒流,柱流量1.0mL/min;进样体积1.0μL;分流进样,分流比5∶1;进样口温度300℃;升温程序为初始温度185℃,保持3min,然后以20℃/min升至245℃,保持17min;EI电离方式,电离能量70eV,离子源温度230℃,传输线温度300℃,溶剂延迟时间为3min,选择离子模式扫描,监测碎片离子:m/z 105(定量离子)、51(定性离子)、77(定性离子)、270(定性离子),结果如图5所示。
上述实施例仅供说明本发明之用,而并非是对本发明专利的限制;应当指出的是,对于本领域的普通技术人员,在不脱离本发明构思的情况下,还可以做出各种变化和变型,这些都属于本发明的保护范围;因此,凡是跟本发明权利要求范围所做的均等变化与修饰,均应属于本发明权利要求的覆盖范围。
Claims (4)
1.一种测定海水中乙二醇含量的气相色谱-质谱检测方法,其特征在于,
(1)仪器条件
1)气相色谱条件
采用色谱柱DB-WAX ms(30mm×0.25mm×0.25μm),恒流,柱流量1.0mL/min;进样体积1.0μL;分流进样,分流比5∶1;进样口温度300℃;升温程序为初始温度185℃,保持3min,然后以20℃/min升至245℃,保持17min;
2)质谱条件
EI电离方式,电离能量70eV,离子源温度230℃,传输线温度300℃,溶剂延迟时间为3min,选择离子模式扫描,特征碎片离子定性定量;
(2)建立标准曲线
称取适量乙二醇标准物质,水溶解并定容,配制成1000.0mg/L的标准储备液,4℃密封储存;量取一定体积的标准储备液,经水稀释,配制成100.0mg/L的标准中间液,4℃密封储存;分别量取适量标准中间液,经水稀释,配制成0.01、0.10、0.50、1.00、2.00、5.00mg/L的系列标准工作液;分别量取5.0mL系列标准工作液,加入10mL蒸馏水,混匀,加入3.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;
依照“(1)仪器条件”分析上述滤液,以目标物定量离子的峰面积为纵坐标,以相应的浓度为横坐标绘制标准曲线;
(3)样品前处理
精确量取5.0mL水样于离心管中,加入1.0mL氢氧化钠溶液,漩涡混匀,5000r/min离心5min,取上清液;在沉淀中加入5mL蒸馏水,漩涡混匀,5000r/min离心5min,取上清液;重复清洗沉淀2次,合并上清液,漩涡混匀,5000r/min离心5min,取清液;
然后在上述清液中加入2.0mL氢氧化钠溶液,漩涡混匀;加入250μL苯甲酰氯,漩涡混匀2min,立即加入2.0mL正己烷,漩涡混匀1min,取上清液,过0.22μm滤膜,供气相色谱-质谱检测;
(4)计算:外标法计算,按以下公式计算试样中目标物的含量:
X=c
上述公式中:
X——试样中待测物的含量,单位为毫克每升(mg/L);
c——样液浓度,单位为毫克每升(mg/L);
注:计算结果保留两位有效数字。
2.根据权利要求1所述的一种测定海水中乙二醇含量的气相色谱-质谱检测方法,其特征在于,定量离子为m/z 105,定性离子为m/z 51、77、270。
3.根据权利要求1所述的一种测定海水中乙二醇含量的气相色谱-质谱检测方法,其特征在于,所述的氢氧化钠溶液浓度为40%(m/v),是将40.0g氢氧化钠溶于100mL水中,搅拌混匀后获得的。
4.根据权利要求1所述的一种测定海水中乙二醇含量的气相色谱-质谱检测方法,其特征在于,该方法的检出限为0.01mg/L。
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