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[液相色谱-质谱联用测定农产品中多果定的分析方法]

[Analytical method of dodine in agricultural products by LC/MS].

作者信息

Aoyagi Mitsutoshi, Niiyama Kazuhito, Takatsuki Satoshi, Nemoto Satoru, Sasaki Kumiko, Maitani Tamio

机构信息

Hokkaido Institute of Public Health, Kita-ku, Sapporo 0600819, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2009 Apr;50(2):58-63. doi: 10.3358/shokueishi.50.58.

Abstract

A method for the determination of dodine in agricultural products was developed by using liquid chromatography-electrospray ionization mass spectrometry (LC/ESI-MS). Dodine was extracted with acetonitrile and then acetonitrile-water (7 : 3) from a sample, and re-extracted with ethyl acetate. The extract was cleaned up on a PSA cartridge column (500 mg), and dodine was analyzed by LC/MS. In the case of oil seeds and nuts, hexane/acetonitrile-hydrochloric acid partition was performed to remove lipids before re-extraction with ethyl acetate. In the case of samples that contained a lot of chlorophyll, the eluate of the PSA cartridge column was further cleaned up on a graphitized carbon cartridge column (500 mg). The calibration curve was linear from 0.0001-0.02 microg/mL of dodine. The recoveries of dodine from sixteen kinds of agricultural products fortified at 0.1 mg/kg were 80.3-100.0%, and their relative standard deviations were 0.3-6.4%. The limits of detection (S/N=3) were 0.0006 mg/kg.

摘要

建立了一种使用液相色谱 - 电喷雾电离质谱法(LC/ESI-MS)测定农产品中多果定的方法。多果定先用乙腈从样品中提取,然后用乙腈 - 水(7:3)提取,再用乙酸乙酯反萃取。提取物在PSA柱(500mg)上净化,多果定通过LC/MS分析。对于油籽和坚果,在用乙酸乙酯反萃取之前,先进行己烷/乙腈 - 盐酸分配以去除脂质。对于含有大量叶绿素的样品,PSA柱的洗脱液在石墨化碳柱(500mg)上进一步净化。多果定的校准曲线在0.0001 - 0.02μg/mL范围内呈线性。在16种添加浓度为0.1mg/kg的农产品中,多果定的回收率为80.3 - 100.0%,相对标准偏差为0.3 - 6.4%。检测限(S/N = 3)为0.0006mg/kg。

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