液相色谱-串联质谱法测定巴沙鱼样品中的氯酸盐和高氯酸盐

Ngoc Lien Huynh Thi, Son Co Hong, Luy Nguyen Van
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摘要

建立了hplc - esi -MS/MS法测定巴沙鱼样品中氯酸盐和高氯酸盐的方法。用1%甲酸酸化的甲醇溶液提取样品中氯酸盐和高氯酸盐的残留物。提取液用C18粉清洗,正相柱分离氯酸盐和高氯酸盐,LC-ESI-MS/MS仪定量。结果表明,该方法特异性好,线性校准曲线在0.0005 ~ 0.015 mg/L范围内;定量限(LOQ)为0.005 mg/kg;回收率为91 ~ 109%,相对标准偏差为6.4 ~ 9.5%,均满足SANTE的要求。将该方法应用于实际分析,共从海产品加工企业采集了427份巴沙鱼鱼片样品。76份样品中检出氯酸盐含量相当于18%。氯酸盐浓度为0.43 ~ 253 mg/kg。
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Determination of chlorate and perchlorate in pangasius samples by liquid chromatography tandem mass spectrometry (LC-MS/MS)
The LC-ESI-MS/MS method has been successfully developed for determination of chlorate and perchlorate in pangasius samples. Residues of chlorate and perchlorate in the sample were extracted with a methanolic solution acidified with 1% formic acid. Then, the extract was cleaned with C18 powder, used a normal phase column to separate chlorate and perchlorate, and quantified on an LC-ESI-MS/MS instrument. The method was validated for good specificity, linear calibration curve in the range of 0.0005 - 0.015 mg/L; the limit of quantification (LOQ) was 0.005 mg/kg; the recovery and relative standard deviation was from 91 to 109% and from 6.4 to 9.5% respectively and all met the requirements of SANTE. The method was applied to the real analysis, a total of 427 pangasius fillet samples collected from seafood processing companies. There were 76 samples were detected chlorate equivalent to 18%. The concentration of chlorate ranged from 0.43 to 253 mg/kg.  
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