高效液相色谱-电感耦合等离子体质谱法测定蚝油类调味品中5种砷形态
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(1.首都医科大学公共卫生学院,北京 100069;2.北京市疾病预防控制中心 食物中毒诊 断溯源技术北京市重点实验室,北京 100013;3.北京市预防医学研究中心,北京 100013)

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陈镇 女 硕士生 研究方向为与健康相关的元素分析E-mail:chenzhen2017@qq.com通信作者:┣┣(中)通信作者┫┫刘丽萍 女 主任技师 研究方向为光谱和质谱E-mail:llp9312@163.com

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Determination of five arsenic species in oyster sauce condiments by high performance liquid chromatography inductively coupled plasma mass spectroscopy
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(1.School of Public Health, Capital Medical University, Beijing 100069, China;2.Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China;3.Beijing Center for Preventive Medicine Research, Beijing 100013, China)

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    摘要:

    目的 采用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP/MS)联用技术对蚝油类调味品中砷甜菜碱(AsB)、亚砷酸根、二甲基砷(DMA)、一甲基砷(MMA)和砷酸根5种砷形态进行分析方法研究。方法 蚝油类样品采用1%硝酸90 ℃热浸提3 h,提取液以8 000 r/min离心10 min,取上清液过0.22 μm水系滤膜。采用Hamilton PRP-X100阴离子交换柱(250 mm×4.1 mm,10 μm),以10和20 mmol/L两种磷酸氢二铵溶液(含2%甲醇)为流动相,梯度洗脱。结果 5种砷形态在0.5~100 μg/L范围内线性良好,相关系数(r)均大于0.999,检出限分别为0.1、0.1、0.1、0.2、0.2 μg/L,加标回收率均在83.2%~103.4%之间,相对标准偏差(RSD)均小于5%。结论 本试验所建方法操作简单,线性范围宽,灵敏度高,适用于蚝油类样品的测定。

    Abstract:

    Objective High-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS) was used to analyze five arsenic species in oyster sauce seasonings, including arsenobetaine (AsB), arsenite As (Ⅲ), dimethyl arsenic (DMA), monomethyl arsenic (MMA) and arsenate As (V). Methods Oyster sauce samples were extracted with 1% nitric acid at 90 ℃ for 3 h, the extract was centrifuged at 8 000 r/min for 10 min, and the supernatant was filtered through 0.22 μm water filtration membrane. A Hamilton PRP-X100 anion exchange column (250 mm×4.1 mm, 10 μm) was used with 10 and 20 mmol/L diammonium hydrogen phosphate methanol solution (containing 2% methanol) as mobile phase for gradient elution. Results The linear range of five arsenic species were good in the range of 0.5-100 μg/L, and the correlation coefficient (r) was above 0.999. The detection limits were 0.1,0.1,0.1,0.2 and 0.2 μg/L, respectively. The recoveries were 83.2%-103.4%, and the relative standard deviations (RSD) were less than 5%. Conclusion The method is simple with a wide linear range and high sensitivity. It is suitable for the determination of oyster sauce samples.

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陈镇,刘丽萍,陈绍占.高效液相色谱-电感耦合等离子体质谱法测定蚝油类调味品中5种砷形态[J].中国食品卫生杂志,2021,33(2):149-154.

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  • 收稿日期:2020-12-11
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  • 在线发布日期: 2021-06-15
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