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    高效液相色谱-电感耦合等离子体质谱法测定畜禽肉中5种砷形态的含量

    Determination of 5 Arsenic Species in Livestock and Poultry Meat by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    • 摘要: 提出了高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定畜禽肉中三价砷As(Ⅲ)、五价砷As(Ⅴ)、二甲基砷(DMA)、一甲基砷(MMA)、砷甜菜碱(AsB)等5种砷形态含量的方法。取样品1.000 g,加入10 mL含1%(体积分数)硝酸的10%(体积分数)甲醇溶液(提取剂),于60 ℃超声提取2.0 h。冷却,离心,分取5 mL上清液,加入5 mL正己烷,振摇1 min,离心10 min,弃去上层正己烷相,再加入5 mL正己烷重复上述步骤1次。吸取下层清液,过0.45 μm有机滤膜。以Agilent ZORBAX SB-Aq色谱柱(250 mm×4.6 mm,5 μm)为分离柱,以含5 mmol·L-1己烷磺酸钠的20 mmol·L-1柠檬酸溶液(pH 4.3)为流动相进行等度洗脱滤液中的目标物。结果表明:5种砷形态标准曲线的线性范围均为2~50 μg·L-1,检出限(3S/N)为0.1~0.2 μg·L-1;对实际样品进行3个浓度水平的加标回收试验,5种砷形态的回收率为81.5%~101%,测定值的相对标准偏差(n=6)为1.3%~3.6%。方法用于10份实际样品分析,其中As(Ⅲ)、DMA和AsB的检出率较高,肝脏、肾脏中的砷形态检出量高于肌肉中的,但均远低于GB 2762—2017对肉及肉制品中总砷的限量(0.5 mg·kg-1)要求。

       

      Abstract: A method for the determination of 5 arsenic species, including of trivalent arsenic As(Ⅲ), pentavalent arsenic As(Ⅴ), dimethylarsenic (DMA), monomethylarsenic (MMA), arsenobetaine (AsB) in livestock and poultry meat by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was proposed. The sample (1.000 g) was taken, and 10 mL of 10% (volume fraction) methanol solution containing 1% (volume fraction) nitric acid (as extractant) was added for extraction by ultrasound at 60 ℃ for 2.0 h. After cooling and centrifugation, an aliquot (5 mL) of the supernatant was taken and 5 mL of n-hexane was added. The mixed solution was shaken for 1 min, and centrifuged for 10 min. The upper n-hexane phase was discard, and 5 mL of n-hexane was added to repeat the above steps once. The lower clear solution was aspirated,and passed through a 0.45 μm filter membrane. Agilent ZORBAX SB-Aq column (250 mm×4.6 mm, 5 μm) was used as the separation column, and 20 mmol · L-1 citric acid solution containing 5 mmol · L-1 sodium hexanesulfonic acid was used as the mobile phase for isocratic elution of targets in the filtrate. It was shown that linear ranges of the standard curves for the 5 arsenic species were 2-50 μg · L-1, with detection limits (3S/N) in the range of 0.1-0.2 μg · L-1. Test for recovery was made on the actual sample by the standard addition method at 3 concentration levels, giving the recovery of 5 arsenic species in the range of 81.5%-101%, and RSDs (n=6) of the determined values were in the range of 1.3%-3.6%. The method was used to analyze 10 actual samples, in which detection rates of As(Ⅲ), DMA and AsB were higher, and the detected amounts of arsenic species in liver and kidney were higher than those in muscle, but they were far lower than the limit (0.5 mg · kg-1) of total arsenic in meat and meat products set by GB 2762—2017.

       

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