干旱区生态环境知识资源中心(Arid): 固相萃取-超高效液相色谱-串联质谱法测定水体中4种解热镇痛类药物

Arid

	固相萃取-超高效液相色谱-串联质谱法测定水体中4种解热镇痛类药物
其他题名	Determination of four antipyretic and analgesic drugs in water by solid-phase extraction coupled ultra-performance liquid chromatography-tandem mass spectrometry
	朱峰; 姚志建; 霍宗利; 吉文亮; 刘华良; 周庆; 李爱民; 焦伟; 谷静
来源期刊	色谱
ISSN	1000-8713
出版年	2020
卷号	38 期号:12
中文摘要	近年来,环境水体中出现的药物及个人护理品污染物受到人们越来越多的关注,其中就包括解热镇痛类药物。传统的固相萃取材料对水体中解热镇痛类药物的富集效率较低。为此,开发了一种亲水亲脂型的双亲多孔吸附聚合物材料(Guochuang hydrophilic material,GCHM)。以N-乙烯基吡咯烷酮和二乙烯基苯为原料,利用乳液胶束-分步反应法成功制备出GCHM。基于自主研发的固相萃取柱,采用超高效液相色谱-串联质谱技术,建立了水体中4种解热镇痛类药物的检测方法。水样经GCHM固相萃取柱富集净化后上机检测,以0.1%(v / v)甲酸水溶液和乙腈作为流动相进行梯度洗脱,目标分析物在ACQUITY UPLC~ HSS T3色谱柱(100 mm*2.1 mm,1.8 mum)上实现分离,在电喷雾正离子模式下进行多反应监测(MRM),内标法定量。比较Oasis HLB、Bond Elut Plexa和GCHM 3种固相萃取柱的富集效率,结果表明GCHM固相萃取柱总体效果最优。在不同pH值下比较了GCHM固相萃取柱对目标分析物的富集效果,并对基质效应进行了评估。结果表明,当pH为7时,4种目标分析物在固相萃取柱上的富集效果最好;各物质的基质效应均在82.8% ~ 102.2%之间,表明水样经GCHM固相萃取柱净化后,基质去除明显。4种目标分析物在1~ 100 mug / L范围内线性关系良好,相关系数(r)均大于0.995,方法定量限(S/ N= 10)在1 ~ 5 ng / L之间,在3个加标水平下的回收率均在85.6% ~ 106.4%之间,相对标准偏差(RSD)均低于5.6%。GCHM固相萃取柱成本低,效果好,适用于水体中4种解热镇痛类药物的检测,较商品化的进口固相萃取柱具有潜在的优势,值得推广应用。
英文摘要	The widespread use of pharmaceutical and personal care products (PPCPs),including antipyretic and analgesic drugs,in the last two decades had led to the existence of PPCP residues in the environment,thus raising concerns about their pseudo-persistent nature and potential threat to human health. Generally,most of the detected contaminants are present at low levels ( ranging from ng / L to mug / L)in environmental water. Therefore,advanced analytical methodologies are crucial to monitor the occurrence and distribution of antipyretic and analgesic drugs in environmental water. However,trace analysis of environmental pollutants is always challenging because it is necessary to extract analytes present in the sample at ultralow levels from complex environmental matrices. Therefore,an appropriate sample pretreatment is necessary to enrich the target compounds. Conventional solid-phase extraction materials show poor efficiency for the enrichment of antipyretic and analgesic drugs. We herein report a hydrophilic and lipophilic amphiphilic porous polymeric material GCHM (Guochuang hydrophilic material). GCHM was successfully prepared by a stepwise emulsification and micellization process using N-vinyl-2-pyrrolidone (NVP)and divinylbenzene (DVB)as raw materials. An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS)method was developed for the determination of four antipyretic and analgesic drugs in water using our solid-phase extraction (SPE)column. The water samples were extracted and purified by the GCHM solid-phase extraction column,and then analyzed by UPLC-MS / MS. Gradient elution was carried out with 0.1% formic acid aqueous solution and acetonitrile as the mobile phase. The target analytes were separated on an ACQUITY UPLC HSS T3 column (100 mm*2.1 mm,1.8 mum),and multiple reaction monitoring (MRM)was conducted in the positive electrospray ionization mode. The isotope internal standard method was used for quantitative correction. Comparison of the enrichment efficiencies of Oasis HLB,Bond Elut Plexa,and GCHM revealed that GCHM showed the best performance. Different pH values affecting the enrichment efficiency of the GCHM SPE column were optimized,and the matrix effect was evaluated. The results showed that the four target analytes gave the best enrichment effect on the SPE column at pH 7,and the matrix effect for each substance was between 82.8% and 102.2%,indicating obvious matrix removal after the water sample was purified by the GCHM SPE column. Good correlation coefficients (r)greater than 0.995 were observed for all the target compounds in the range of 1-100 mug / L. The method limits of quantitation (S / N= 10)ranged from 1 ng / L to 5 ng / L. The corrected recoveries were 85.6% to 106.4%,and the relative standard deviations (RSD)were under 5.6%. The GCHM solid-phase extraction column is inexpensive and efficient,being suitable for the detection of the four antipyretic and analgesic drugs in water. Subsequently,the occurrence of these selected antipyretic and analgesic drugs in water samples from Shanghai,Jiangsu,and Guangdong provinces were studied. The GCHM column has potential advantages over the commercial imported SPE column and is worthy of widespread application. This column can also aid the enrichment and purification of other compounds with similar structures or properties in water.
中文关键词	固相萃取 ; 超高效液相色谱-串联质谱 ; 解热镇痛类药物 ; 水体
英文关键词	solid-phase extraction (SPE) ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) antipyretic and analgesic drugs water
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6902137
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353722
作者单位	朱峰, 江苏省疾病预防控制中心, 南京, 江苏 210009, 中国. 霍宗利, 江苏省疾病预防控制中心, 南京, 江苏 210009, 中国. 吉文亮, 江苏省疾病预防控制中心, 南京, 江苏 210009, 中国. 刘华良, 江苏省疾病预防控制中心, 南京, 江苏 210009, 中国. 谷静, 江苏省疾病预防控制中心, 南京, 江苏 210009, 中国. 姚志建, 南京大学环境学院;;江苏国创环保科技有限公司, 污染控制与资源化研究国家重点实验室;;, 南京;;南京, ;; 210023;;211100. 焦伟, 南京大学环境学院;;江苏国创环保科技有限公司, 污染控制与资源化研究国家重点实验室;;, 南京;;南京, ;; 210023;;211100. 周庆, 南京大学环境学院, 污染控制与资源化研究国家重点实验室, 南京, 江苏 210023, 中国. 李爱民, 南京大学环境学院, 污染控制与资源化研究国家重点实验室, 南京, 江苏 210023, 中国.
推荐引用方式 GB/T 7714	朱峰,姚志建,霍宗利,等. 固相萃取-超高效液相色谱-串联质谱法测定水体中4种解热镇痛类药物[J],2020,38(12).
APA	朱峰.,姚志建.,霍宗利.,吉文亮.,刘华良.,...&谷静.(2020).固相萃取-超高效液相色谱-串联质谱法测定水体中4种解热镇痛类药物.色谱,38(12).
MLA	朱峰,et al."固相萃取-超高效液相色谱-串联质谱法测定水体中4种解热镇痛类药物".色谱 38.12(2020).