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蚕蛹是极富营养价值的昆虫食品资源。建立精准、快速、稳定检测蚕蛹中金属元素的技术,是完善蚕蛹质量检测与食用安全风险评估技术体系的一个重要组成部分。采用HNO3+H2O2体系对家蚕蛹和柞蚕蛹样品进行微波消解,再结合电感耦合等离子体质谱(ICP-MS)法,测定11份家蚕蛹样品和2份柞蚕蛹样品中钾、钠、镁、钙、铁、锌、锰、镍、铜、铷、镉、铅等12种金属元素的含量。在优化的仪器工作条件下,12种元素的检出限为0.02~66.41μg/L,相对标准偏差均<3.87%,加标回收率在87.1%~107.7%之间。检测结果表明家蚕蛹和柞蚕蛹中均含有丰富的钾、钠、钙、镁、铁、锌、铜、锰等对人体有益的元素,有害元素镉的含量均较低,但有2个柞蚕蛹样品和2个家蚕蛹样品中的铅含量较高。检测方法学验证试验表明,微波消解结合ICP-MS法具有良好的准确度和精密度,能满足对蚕蛹样品中常量元素和微量元素同时检测的需要;对11份家蚕蛹样品和2份柞蚕蛹样品的检测结果初步提示,一些家蚕和柞蚕饲养区在一定程度上受到了重金属铅的污染。
Silkworm pupae are highly nutritious insect food resources. The establishment of accurate, rapid and stable detection of silkworm chrysalis in the metal element technology, is to improve the pupa quality inspection and food safety risk assessment technology system is an important part. The samples of silkworm pupae and tussah pupae were subjected to microwave digestion with HNO3 + H2O2 system. Combined with inductively coupled plasma mass spectrometry (ICP-MS), the contents of potassium, sodium, magnesium and calcium in 11 samples of silkworm pupae and 2 samples of tussah pupae were determined , Iron, zinc, manganese, nickel, copper, rubidium, cadmium, lead and other content of 12 kinds of metal elements. The detection limits of the 12 elements were 0.02 ~ 66.41 μg / L with the relative standard deviations of <3.87% and the spiked recoveries of 87.1% ~ 107.7% under the optimized instrument working conditions. The results showed that both silkworm pupae and tussah pupae were rich in potassium, sodium, calcium, magnesium, iron, zinc, copper, manganese and other beneficial elements to human body, with the content of harmful elemental cadmium being low, but there were two tupa pupae Samples and two silkworm pupa samples had higher levels of lead. The validation of the test method showed that the microwave digestion coupled with ICP-MS method had good accuracy and precision, which could meet the need of simultaneous detection of trace elements and trace elements in silkworm pupae samples. In 11 samples of silkworm pupae and 2 samples of tussah pupae The results of the sample preliminary suggested that some silkworm and tussah breeding areas were to some extent contaminated by heavy metal lead.