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土壤磺胺类抗生素固相萃取-高效液相色 谱法的构建与优化
刘潇雅, 徐源洲, 贺南南, 李辉信, 胡锋, 徐莉
南京农业大学资源与环境科学学院
摘要:
设计正交试验对红壤中磺胺甲恶唑(sulfamethoxazole, SMZ)的萃取方法进行优化,并结合高效液相色谱,构建了固相萃取-高效液相色谱联合测定法(SPE-HPLC),并将该方法应用于不同抗生素以及不同类型土壤中SMZ的提取测定。结果表明,在以乙腈-磷酸盐缓冲液为提取液、提取液量为10 ml、超声时间为15 min、9 ml甲醇淋洗固相萃取柱(HLB)的条件下,红壤中SMZ的提取效果最优,0.25 mg/kg的SMZ回收率达到85.58%,能够满足环境样品的分析要求。利用该法提取测定红壤中不同抗生素包括3种磺胺类抗生素(磺胺嘧啶、磺胺二甲基嘧啶、磺胺甲基嘧啶)和2种四环素类抗生素(土霉素、盐酸四环素),结果表明,当抗生素浓度为0.25 mg/kg时,磺胺类抗生素(SAs)的回收率范围在67.31% ~ 85.58%,四环素类抗生素(TCs)的回收率范围在20.81% ~ 59.33%。利用该法分别提取测定不同类型土壤中的SMZ回收率,得到潮土中SMZ的回收率最大,达到92.92%,其次为荒漠土、红壤、紫色土,最低的回收率出现在黄棕壤,仅为53.62%。据相关性分析表明,回收率与土壤电导率(EC)、微生物碳氮比(C/N)呈极显著负相关(P<0.01),与阳离子交换量(CEC)、有机质(SOM)呈显著负相关(P<0.05)。
关键词:  土壤  固相萃取  高效液相色谱  正交试验  磺胺类  四环素类
DOI:10.13758/j.cnki.tr.2019.06.012
分类号:X830.2
基金项目:中央高校基本科研业务费专项资金(KYZ201626),公益性行业(农业)科研专项经费项目(201503121)和中国博士后科学基金面上项目(2016M591856)资助。
Optimization and Detecting Sulfamethoxazole in Soils Using Solid Phase Extraction-High Performance Liquid Chromatography
LIU Xiaoya, XU Yuanzhou, HE Nannan, LI Huixin, HU Feng, XU Li
Nanjing agricultural university
Abstract:
In this paper, an orthogonal experiment was designed to optimize the extraction method of sulfamethoxazole (SMZ) in red soil and a solid phase extraction-high performance liquid chromatography (SPE-HPLC) method was built for SMZ detection. The method was used to determine different antibiotics including SMZ from different soils. The results showed that the optimal extraction conditions for SMZ in the red soil was 10 ml acetonitrile-phosphate buffer as the extracting solution, ultrasonic oscillation time for 15 min and 9 ml methyl alcohol elution. The recovery of 0.25 mg/kg SMZ was 85.58%, indicating this method applicable for the environmental sample analysis. Meanwhile, this method was used to extract other antibiotics, including three sulfa antibiotics (sulfadiazine, sulfamerazine, sulfadimidin) and two tetracycline antibiotics (oxytetracycline, tetracycline), the average recoveries of 0.25 mg/kg sulfas and tetracyclines were 67.31%-85.58% and 20.81%-59.33%. Under HPLC with UV detection, the detection limit of SMZ was 2.38 μg/kg, showed a good accuracy. Simultaneously, the detection limits of sulfa and tetracycline antibiotics were between 2.38-12.57 μg/kg, indicating this method better suited to detect sulfa antibiotics in soil according to the laboratory quality control standard. Besides, the method was also used to test SMZ recoveries from different soil types, the largest SMZ recovery rate (92.92%) was obtained in fluvo-aquic soil, followed by desert soil, red soil and purple soil, while the lowest recovery rate (53.62%) were in yellow-brown soil. The correlation analysis showed that a significant negative correlation between recovery rate and soil EC, C/N (P<0.01), and CEC, SOM (P<0.05).
Key words:  Soil  Solid-phase extraction  High performance liquid chromatograph  Orthogonal experiment  Sulfonamide  Tetracycline

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