摘要
建立了高效液相色谱（HPLC）-串联紫外检测法检测有机肥中洛克沙胂的分析方法。选用20g·L-1K2HPO4作为提取剂,于60℃温度下超声提取有机肥中的洛克沙胂,采用MAX固相萃取柱净化。结果表明,采用Symmetry ShieldTMRP 18色谱柱,以含0.1%甲酸的0.05mol·L-1 KH2PO4∶甲醇=95∶5（V/V）溶液作流动相,等度洗脱,紫外266nm检测,洛克沙胂的保留时间短,且可完全避开杂质峰的干扰;其平均加标回收率介于81.14%~82.75%之间,相对标准偏差（RSD）〈7.0%,检出限为20μg·L-1。方法重现性好,精密度高,操作简便,适用于有机肥中洛克沙胂检测。
A high-performance liquid chromatography（HPLC）method with UV detection was developed for the determination of roxarsone in animal manure.The results showed that the retention time of roxarsone was short,and it could completely avoid the interference of miscellaneous peak through the Symmetry ShieldTMRP 18 column when using the solution of 0.05mol·L-1 KH2PO4：methanol=95∶5（V/V）containing 0.1%formic acid as the mobile phase at the isocratic elution.20g·L-1 K2HPO4 was chosen as the extracting agent to extract the roxarsone in the manure under the ultrasound conditions at60℃,and the samples were further purified by solid phase extraction（SPE）on MAX cartridges.The average recoveries ranged from 81.14% to 82.75% with relative standard deviations（RSD）less than7.0%,the coefficient of variation between 0.053% and 2.04% and the detection limit is 20μg·L-1.What＇s more,it had advantages of good reproducibility,high precision and ease of operation.This method is applicable to detect roxarsone in manure.
出处
《分析科学学报》
CAS
CSCD
北大核心
2015年第1期127-130,共4页
Journal of Analytical Science
基金
上海市自然科学基金(No.12ZR1420200)
国家质检公益性行业科研专项(No.201310269)
上海市科委重点支撑项目(No.13231202900)
关键词
高效液相色谱法
有机肥
洛克沙胂
High-performance liquid chromatography
Manure
Roxarsone
Detection
Purification
