高效液相色谱法测定元参、黄芩和杭白菊中的 多菌灵残留
Determination of carbendazim residue in Radix Scrophulariae, Radix Scutellariae and Flos Chrysanthemi by high performance liquid chromatography
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摘要: 建立了一种测定元参、黄芩和杭白菊3种中药材中多菌灵残留的反相高效液相色谱分析方法(R-HPLC)。样品用丙酮提取,柱层析(弗罗里硅土-中性氧化铝=7∶ 4,质量比)和液液分配净化,以甲醇-水(体积比60∶ 40)为流动相,在波长281 nm下对待测组份进行检测,外标法定量。结果表明,多菌灵在3种中药材中的添加回收率分别为元参:69.08% ~88.31%,相对标准偏差(RSD)为3.35% ~4.67%;黄芩:71.39% ~88.40%,RSD为3.73% ~8.62%;杭白菊:73.33% ~97.31%,RSD为2.83% ~9.44%;均符合农药残留分析的要求。该杀菌剂在0.05~10 mg/L之间具有良好的线性关系,r=0.999 7,仪器的最小检出量(按S/N=3计)分别为0.3、0.5和0.3 ng,方法的最低检测浓度分别为0.01、0.05和0.01 mg/kg。该方法简单易行,净化效果较好,适合各种中药材中多菌灵残留的检测。Abstract: A reversed phase high-performance liquid chromatography(HPLC) method has been developed for carbendazim residue in Radix Scrophulariae,Radix Scutellariae and Flos Chrysanthemi.Carbendazim was extracted with acetone,cleaned up by column chromatography(florisil-neutral alumina=7∶ 4,m/m) and followed by liquid-liquid partition.HPLC conditions were as follows:Diamonsil C18(2) column with temperature at 30℃,methanol-water(60∶ 40,V/V) as mobile phase with flow rate of 0.8 mL/min and the detection wave length at 281 nm.The fortified recoveries and relative standard deviation(RSD) were from 69.08% to 88.31% and 3.35% to 4.67% in Radix Scrophulariae,from 71.39% to 88.40% and 3.73% to 8.62% in Radix Scutellariae,from 73.33% to 97.31% and 2.83% to 9.44% in Flos Chrysanthemi.The standard curve of carbendazim was linear in the range of 0.05-10 mg/L(r=0.999 7),the limit of detection(S/N=3) was 0.3,0.5 and 0.3 ng,the limit of quantification was 0.01,0.05 and 0.01 mg/kg,respectively.The analytical method is easier,faster,satisfied with the analysis of carbendazim residue in three kinds of Chinese herbal medicines and has better purification effect.