A pretreatment method for HPLC analysis of cypermethrin in microbial degradation systems.
A pretreatment method for HPLC analysis of cypermethrin in microbial degradation systems.
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DOI：
10.1093/chromsci/bms030
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发表时间：
2012-07
影响因子：
1.3
通讯作者：
Shuliang Liu;K. Yao;Dongying Jia;Nan Zhao;W. Lai;Huaiyu Yuan
中科院分区：
文献类型：
--
作者：
Shuliang Liu;K. Yao;Dongying Jia;Nan Zhao;W. Lai;Huaiyu Yuan
针对高效液相色谱法测定微生物降解体系中氯氰菊酯（CY）浓度时，由于CY在体系中分布不均匀而导致测定结果不准确的问题，系统研究了高效液相色谱法测定微生物降解体系中CY的前处理方法。建立了CY的前处理方法，包括样品的采集、提取和脱水。部分取样可用于细菌和酵母系统，其中CY被乳化剂均匀分散，而总取样仅适用于有或无乳化剂的霉菌系统。在超声波条件下，用乙腈超声破碎微生物细胞后，样品中的CY可被完全提取。提取液经无水Na（2）SO（4）柱层析后，用乙腈洗脱，可有效地进行脱水和纯化。用HPLC法测定前处理样品中CY的含量，精密度高（RSD = 1.14%，n = 5），稳定性好（RSD = 1.57%，n = 5）。微生物降解体系中3个不同加标水平的回收率为95.68 ~ 108.09%（RSD = 0.50- 5.87%，n = 5）。
In this paper, a pretreatment method for high-performance liquid chromatography (HPLC) determination of cypermethrin (CY) in microbial degradation systems was systemically studied, primarily to solve the problem of inaccurate determination of CY concentration caused by its uneven distribution in the systems. A suitable pretreatment method was established, including sampling, extraction and dehydration of CY. Partial sampling could be taken for bacterial and yeast systems in which CY was uniformly dispersed by an emulsifying agent, while total sampling was only suitable for mold systems with or without an emulsifying agent. CY could be fully extracted from the samples in which microbial cells were disrupted by ultrasonic treatment with acetonitrile under ultrasonic condition. The extract could be effectively dehydrated and purified by passing it through an anhydrous Na(2)SO(4) column followed by an elution with acetonitrile. The determination of CY in the pretreated sample by HPLC showed a high precision [relative standard deviation (RSD) = 1.14%, n = 5] and a good stability over a period of five days (RSD = 1.57%, n = 5). The recoveries of CY in microbial degradation systems at three different spiked levels ranged from 95.68 to 108.09% (RSD = 0.50-5.87%, n = 5).