摘要
取饮用水样1.0L,用0.2μm滤膜过滤。滤液以5mL·min^-1的流量通过活化后的HLB固相萃取柱(SPE),使18种被测物在柱上分离富集。先后用水10mL和15%(体积分数)甲醇溶液10mL淋洗HLB柱,随即用甲醇15mL洗脱吸附于柱上的被测物。收集洗脱液并于30℃下吹氮,使其体积蒸缩至200μL,加水定容至1.0mL,离心10min,取其上清液,用0.22μm针式过滤器过滤后,取其滤液在仪器工作条件下进行超高效液相色谱-串联质谱(UPLC-MS/MS)分析。选用Waters UPLCTMBEH C18色谱柱作为分离柱,用不同比例的(A)8mmol·L^-1甲酸铵溶液[含0.1%(体积分数,下同)甲酸]和(B)体积比为1∶1甲醇-乙腈混合液(含1%甲酸)的混合液作为流动相,将色谱柱上的被测物进行梯度洗脱,18种分析物可在34min内达到较好的分离。在MS/MS分析中选择电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式进行测定。所涉及18种被测物的质量浓度均在15μg·L^-1内与其对应的色谱峰面积呈线性关系,其检出限(3S/N)为5~50pg·L^-1。以超纯水和自来水为基质进行加标回收试验,回收率分别为64.4%~113%和78.2%~116%,测定值的相对标准偏差(n=5)分别为1.6%~19%和2.8%~18%。对采自全国不同区域的7个水厂的实样按方法进行分析,其中有3份水样中检出4-乙酰氨基安替比林的含量高于1ng·L^-1;在所测7份水样中均测得卡马西平和吡喹酮,其含量均低于1ng·L^-1;还在3~5份水样中测得含量1ng·L^-1的四咪唑、磺胺甲恶唑、磺胺噻唑和磺胺二甲基嘧啶等化合物。
1.0L of drinking water sample was taken and filtered through 0.22μm filtering membrane,and the filtrate was passed through the activated HLB SPE column at a flow-rate of 5mL·min^-1 to have the 18typical pharmaceutical and personal-care products(PPCPs)enriched and separated on the SPE column.The column was then rinsed with 10mL of water and 10mL of 15%(φHCOOH)methanol solution successively.The 18analytes were eluted from the SPE column with 15mL of methanol and the eluate was collected and evaporated to ca.200μL by N2-blowing at 30℃.Water was added to the residue to make its volume to 1.0mL,and after centrifugation for 10min,the supernatant was taken and filtered through an injection filter,and the filtrate was used for UPLC-MS/MS analysis under the instrumental working conditions.Waters UPLCTM BEH C18 column was used for chromatographic separation with mobile phase mixtures composing of(A)8 mmol·L^-1 HCOONH4solution[0.1%formic acid(volume fraction,the same below)]and(B)mixture of CH3OH-CH3CN at a volume ratio of 1∶1(1%formic acid)in various proportions,to elute the 18analytes from the chromatographic column by gradient elution.The 18analytes were well saparated within 34min.ESI+mode and MRM mode were adopted in MS/MS determination.Linear relationships between values of peak areas and mass concentration of the 18analytes were found in the same range within 15μg·L^-1.Values of detection limit(3S/N)found were in the range from 5 to 50pg·L^-1.Recovery tests were made by standard addition method using extrapure water and tap water as matrixes,giving results of recovery in the ranges of 64.4%-113%and 78.2%-116%respectively,and values of RSDs(n=5)found were ranged from 1.6%to 19%(for extrapure water)and from 2.8%to 18%(for tap water).Drinking water samples were collected from 7water works in various regions of our country,and were analyzed by the proposed method.4-Acetylaminoantipyrine with contents over 1ng·L^-1 were found in 3of the 7samples;carbamazepine and praziquantel in amounts lower than 1ng·L^-1 w
作者
沈璐
殷浩文
刘敏
王樱芝
SHEN Lu;YIN Haowen;LIU Min;WANG Yingzhi(Bioassaya-Safety Assessment Laboratory,Shanghai Academy of Public Measurement,Shanghai 201203,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2020年第6期641-649,共9页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
上海市卫生体系建设第四轮三年行动计划重点学科建设项目(15GWZK0201)。
