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高效液相色谱-电化学检测法测定猪肉和猪肝中盐酸克伦特罗残留量

Determination of residual clenbuterol in pork meat and liver by HPLC with electrochemical detection.

作者信息

Zhang Xue-zhu, Gan Yi-ru, Zhao Fu-nian

机构信息

Department of Biochemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China.

出版信息

Yao Xue Xue Bao. 2004 Apr;39(4):276-80.

Abstract

AIM

To detect the residual clenbuterol in pork meat and liver using HPLC with Coulometric electrode array system.

METHODS

Homogenized meat or liver sample was treated with 1 mol x L(-1) hydrochloric acid and centrifuged, the fat existing in meat or liver tissue was removed by diethyl ether. The pH of the remaining aqueous layer was adjusted to 10.8 +/- 0.2 or 11.6 +/- 0.2 for meat or liver and liquid-liquid extraction with diethyl ether was followed. The ether extract was evaporated to dryness, the residue was dissolved in the mobile phase. The mobile phase A consisted of 50 mmol x L(-1) phosphoric acid-30 mmol x L(-1) triethylamine and was adjusted to pH 4.0 with 2 mol x L(-1) sodium hydroxide solution. The mobile phase B consisted of methanol-acetonitrile (30:45). A mixture of mobile phase A and B (80:20) was used in the method. A four electrode array module was selected for quantitation, the electrode potentials were set at 450, 600, 650 and 680 mV respectively.

RESULTS

The two calibration curves for meat and liver showed good linearity between 1.88 - 60.16 ng x g(-1), the detection limit of clenbuterol was 1.2 ng x g(-1).

CONCLUSION

This method using HPLC-electrochemical detection is reproducible, and the sensitivity is good enough for the determination of clenbuterol in meat and liver.

摘要

目的

采用带电量检测电极阵列系统的高效液相色谱法检测猪肉和猪肝中的克伦特罗残留量。

方法

将匀浆后的肉或肝样品用1mol·L⁻¹盐酸处理并离心,用乙醚去除肉或肝组织中存在的脂肪。将剩余水相的pH值调至肉样为10.8±0.2、肝样为11.6±0.2,然后用乙醚进行液液萃取。将乙醚萃取液蒸发至干,残渣溶于流动相。流动相A由50mmol·L⁻¹磷酸-30mmol·L⁻¹三乙胺组成,并用2mol·L⁻¹氢氧化钠溶液调至pH4.0。流动相B由甲醇-乙腈(30:45)组成。该方法采用流动相A和B的混合液(80:20)。选择四电极阵列模块进行定量分析,电极电位分别设定为450、600、650和680mV。

结果

肉和肝的两条校准曲线在1.88 - 60.16ng·g⁻¹之间呈良好线性,克伦特罗的检测限为1.2ng·g⁻¹。

结论

该高效液相色谱-电化学检测方法具有重现性,灵敏度足以用于测定肉和肝中的克伦特罗。

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