HPLC-DAD法测定2种阿苯达唑伊维菌素制剂中非法添加非泼罗尼

Determination of illegal fipronil supplementation in two albendazole and ivermectin preparations by HPLC-DAD

建立了2种阿苯达唑伊维菌素制剂中非法添加非泼罗尼的HPLC-DAD检测方法。液相色谱条件为:采用C18(3.5μm,4.6×100 mm)色谱柱;以乙腈-水为流动相,梯度洗脱,流速1.0 mL/min;二极管阵列检测器检测,采集波长范围190~400 nm,记录色谱图波长为220 nm,柱温30℃,进样量10μL。通过液相色谱峰保留时间、峰纯度检查和光谱相似度检查对非法添加物进行确证。结果表明:非泼罗尼质量浓度在0.5~100.0 mg/L范围内与峰面积线性关系良好(r=0.999 92),在2种制剂中非泼罗尼的平均回收率分别在97.85%~99.26%(n=6)和97.47%~99.49%(n=6)之间,RSD均小于3%。本方法高效、简便、准确、可靠,适用于检测以上2种制剂中非法添加的非泼罗尼。

A HPLC-DAD method was established here for the determination of illegal fipronil supplementation in two albendazole and ivermectin preparations.The HPLC conditions were the chromatography column C18 of 3.5μm and 100 mm×4.6 mm;the mobile phase of water and acetonitrile at gradient elution at a flow rate of 1.0 mL/min;a diode array detector with a wavelength range of 190 nm^400 nm and a recorded wavelength of 220 nm;a column temperature of 30℃;and an injection volume of 10μL.Retention time,peak purity test and spectrum similar test were used to confirm the existence of fipronil in the preparations.The results showed that fipronil and other materials were effectively isolated.There was a good linear relationship between the concentration of fipronil and the peak area within the range of 10.0 to 100.0 mg/L(r=0.999 92).The average recoveries of fipronil in the two kinds preparations were 97.85%~99.26%(n=6)and 97.47%~99.49%(n=6),and the inter-batch variation coefficients were less than 3%.In conclusion,the present method was of high-efficiency,convenient application,accuracy and reliability in determination of illegal supplementation of fipronil in the two preparations studied here.