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尿中十六种磺胺类抗菌药物残留量液相色谱串联质谱法测定
其他题名Determination of 16 sulfonamide antibiotics residues in human urine with liquid chromatography-tandem mass spectrometry
李宏亮; 詹铭; 郝莉鹏
来源期刊中国公共卫生
ISSN1001-0580
出版年2019
卷号35期号:7页码:918-921
中文摘要目的建立同时测定尿液中16种磺胺类抗菌药物多残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。方法尿液经酶解处理后,Oasis PRiME HLB(200mg、6mL)固相萃取柱净化,采用Waters BEH C18色谱柱(2.1*100mm,1.7mum),水(含0.01mol/L乙酸铵)和甲醇(含0.01mol/L乙酸铵)作为流动相进行梯度洗脱,电喷雾离子源电离,正离子扫描,多反应监测模式(MRM)进行定性和定量分析。结果16种磺胺类抗菌药物的线性范围为5~1000ng/mL,相关系数均大于0.99。方法定量下限为5ng/mL,检出限为0.3~1.7ng/mL,3个加标水平回收率为71.6%~97.3%,相对标准偏差(RSD)为1.4%~11.7%。结论超高效液相色谱-串联质谱法操作简便、具有较高的灵敏度、特异度和精确性,适用于尿中多种痕量磺胺类抗菌药物残留量的同时测定。
英文摘要Objective To develop a confirmative method detecting 16 sulfonamide antibiotics residues in human urine simultaneously with ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS).Methods Urine samples were analyzed following incubation with beta-glucuronidase,and then purified with an Oasis PRiME HLB (200 mg,6 mL) solid-phase extraction (SPE) cartridge.The UPLC separation was performed on an Waters BEH C18 column (2.1*100 mm,1.7 mum) utilizing a gradient elution program of methanol (containing 0.01 mol/L ammonium acetate) and water (containing 0.01mol/L ammonium acetate) as the mobile phase.Identification and quantification were achieved using electrospray ionization (ESI) in positive mode with multiple reaction monitoring (MRM).Results Good linearities of the analyses were achieved over the concentration of 5-1 000 ng/mL,with the correlation coefficients above 0.99.The method quantitation limits (MQL) for target compounds were 5 ng/mL.The detection limits of the method were 0.3-1.7 ng/mL.Average recoveries of 16 analytes at three spiked levels ranged from 71.6% to 97.3% with the relative standard deviations (RSDs) of 1.4%-11.7%.Conclusion The established UPLC-MS/MS method is of simplify operation and high sensitivity,selectivity and precision,and is applicable to the measurement of trace amounts of sulfonamide antibiotics residues in human urine.
中文关键词尿液样本 ; 磺胺类抗菌药物 ; 残留量 ; 超高效液相色谱串联质谱(UPLC-MS/MS)
英文关键词urine sample sulfonamide antibiotics residue ultra performance liquid chromatography coupled with tandem mass spectrometry
语种中文
国家中国
收录类别CSCD
WOS类目PHARMACOLOGY PHARMACY
WOS研究方向Pharmacology & Pharmacy
CSCD记录号CSCD:6529835
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/239733
作者单位上海市浦东新区疾病预防控制中心复旦大学浦东预防医学研究院, 上海 200136, 中国
推荐引用方式
GB/T 7714
李宏亮,詹铭,郝莉鹏. 尿中十六种磺胺类抗菌药物残留量液相色谱串联质谱法测定[J],2019,35(7):918-921.
APA 李宏亮,詹铭,&郝莉鹏.(2019).尿中十六种磺胺类抗菌药物残留量液相色谱串联质谱法测定.中国公共卫生,35(7),918-921.
MLA 李宏亮,et al."尿中十六种磺胺类抗菌药物残留量液相色谱串联质谱法测定".中国公共卫生 35.7(2019):918-921.
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