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气相色谱-质谱联用法测定两面针根中有机氯农药残留量

[Determination of organochlorine pesticide residues in the roots of Zanthoxylum nitidum by GC-MS].

作者信息

Jiao Ai-Jun, Feng Jie, Lai Mao-Xiang

机构信息

School of Pharmaceutical Sciences, Guangxi Medical University, Nanning 530021, China.

出版信息

Zhong Yao Cai. 2013 Apr;36(4):528-31.

PMID:24133993
Abstract

OBJECTIVE

To determine the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum and provide scientific foundation for the quality control and standard establishment.

METHODS

GC-MS method with selected ion monitoring (SIM) mode was used to analyze the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum. The samples were extracted with acetone and ultrasonic vibrations, and the analytical samples were purified by anhydrous sodium sulfate-anhydrous magnesium sulfate -PSA -C18-PestiCarb -phase extraction (SPE) cartridge.

RESULTS

Eight kinds of organochlorine pesticide were detected simultanously. Small amounts of OP-DDT were detected in samples 1, 4, 5, 6, 11 and 12, no organochlorine pesticide residue was detected in other samples. The RSD of precision ranged from 0.89% to 2.21%, and the average recovery ranged from 85.33% to 103.70%, with the RSD less than 4%.

CONCLUSION

The contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum are less than 0.2 ppm. This method is sensitive, good purifying, and suitable for analyzing organochlorine pesticide residues in the roots of Zanthoxylum nitidum.

摘要

目的

测定两面针根中有机氯农药残留量,为其质量控制和标准制定提供科学依据。

方法

采用气相色谱 - 质谱联用仪,选择离子监测(SIM)模式分析两面针根中有机氯农药残留量。样品用丙酮提取并超声振荡,分析样品经无水硫酸钠 - 无水硫酸镁 - PSA - C18 - PestiCarb 固相萃取(SPE)小柱净化。

结果

同时检测出8种有机氯农药。在样品1、4、5、6、11和12中检测到少量的OP - DDT,其他样品未检测到有机氯农药残留。精密度的相对标准偏差(RSD)为0.89%~2.21%,平均回收率为85.33%~103.70%,RSD小于4%。

结论

两面针根中有机氯农药残留量小于0.2 ppm。该方法灵敏度高、净化效果好,适用于两面针根中有机氯农药残留量的分析。

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