大连地区水库中116种药物与个人护理品的高效液相色谱-四极杆/静电场轨道阱高分辨质谱筛查与测定分析  

Screening and determination of 116 pharmaceuticals and personal care products in reservoirs in Dalian area by high performance liquid chromatography-quadrupole/field orbitrap high resolution mass spectrometry

作　　者：褚莹倩 刘水琳 齐欣 陈溪 周艺蓉 孙韬智 朱乾琨 CHU Yingqian;LIU Shuilin;QI Xin;CHEN Xi;ZHOU Yirong;SUN Taozhi;ZHU Qiankun(Technology Center of Dalian Customs,Dalian,116000,China;Dalian Ecological and Environmental Affairs Service Center,Dalian,116000,China)

机构地区：[1]大连海关技术中心,大连116000 [2]大连生态环境事务服务中心,大连116000

出　　处：《环境化学》2021年第10期3066-3081,共16页Environmental Chemistry

基　　金：大连市科技创新基金(2019J13SN122);国家自然科学基金青年基金(21705065);大连海关科研项目(2021DK18)资助。

摘　　要：采用固相萃取技术对大连地区青云河水库、石门子水库、大渔沟水库、北大河水库水样进行富集净化,通过高效液相色谱-四极杆/静电场轨道阱高分辨质谱对水样中116种药物与个人护理品(pharmaceuticals and personal care products,PPCPs)进行筛查检测与定量分析.结果表明,116种PPCPs化合物在10—100 ng·mL^(-1)范围内线性良好,相关系数R2均在0.99以上,定量限(LOQ)为0.4μg·L^(-1),回收率为40.7%—121.6%.研究发现,水样中激素类化合物能够被普遍检出,其浓度总量范围为1.79—9.33 ng·L^(-1),醋酸泼尼松、醋酸氟氢可的松、醋酸可的松、醋酸氢化可的松和甲基泼尼松龙醋酸酯在4个水库中均有检出,其中醋酸泼尼松和醋酸氟氢可的松在8个采样点位均有检出,为检出频率最高的化合物.大渔沟水库中醋酸泼尼松的检出浓度最大,其检出浓度为1.84 ng·L^(-1).大渔沟水库中激素类化合物的整体污染水平要略高于青云河水库、石门子水库和北大河水库,分析其原因主要受水库的规模、功能类型影响.与国内其他饮用水源地、河流相比较,本研究中4个水库水样中激素类化合物的检出浓度相比较低,属于低等污染水平.Water samples in Qingyunhe Reservoir, Shimenzi Reservoir, Dayugou Reservoir and Beidahe Reservoir of Dalian area were concentrated and cleaned up with solid phase extraction.Totally 116 kinds of pharmaceuticals and personal care products(PPCPs) were screened and quantitated using high performance liquid chromatography-quadrupole/field orbitrap high resolution mass spectrometry. Results showed that the calibration curves of the 116 PPCPs showed good linearity in the range of 10—100 ng·mL^(-1) with correlation coefficients larger than 0.99. The limits of quantitation(LOQ) for the 116 PPCPs were 0.4 μg·L^(-1). The recoveries of these PPCPs were in the range of 40.7%—121.6%. The study indicated that steroid hormones could be widely detected in the water samples with total concentrations ranging from 1.79 ng·L^(-1) to 9.33 ng·L^(-1). Prednisone 21-acetate, fludrocortisone 21-acetate, cortisone 21-acetate, hydrocortisone 21-acetate, and methylprednisolone 21-acetate were detected in the four reservoirs, among which prednisone 21-acetate and fludrocortisone 21-acetate were detected in all the eight sampling sites with the highest frequency. A highest concentration of 1.84 ng·L^(-1) for prednisone 21-acetate was detected in Dayugou Reservoir. The overall pollution of steroid hormones in Dayugou Reservoir was a little higher than that in the other three reservoirs, which was mainly attributed to the scale and function type of the reservoir. Comparing with the reported concentrations in other domestic drinking water and rivers in China, the concentrations of steroid hormones in the four reservoirs in this study were at low levels,which presented the low pollution level.

关 键 词：药物与个人护理品 高分辨质谱 筛查 水库 大连 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]