Method for detecting residual quantity of sodium nitrophenol in aquatic product

Abstract

The invention discloses a method for detecting residual quantity of sodium nitrophenol in an aquatic product and belongs to the technical field of detection of aquatic products. The method comprises the following steps of: extracting and purifying a sample; drawing a standard curve; and determining and quantifying apparatus conditions. According to the method disclosed by the invention, an APCI (Atmosphere Pressure Chemical Ionization) ion source is selected by a mass spectrometer, so that the sensitivity of sodium orotho-nitrophenolate is improved by dozens of times; neutral alumina is adopted for purifying, so that interfering substances such as fat in the sample can be effectively removed, and the concentration time is shortened; sodium hydroxide is added during the concentration process, so that the sodium orotho-nitrophenolate exits in the sample in the form of sodium salt, thereby enabling the recovery rate of the sodium orotho-nitrophenolate to be more than 70%. Phosphoric acid is added after the concentration for neutralizing the excessive sodium hydroxide, so that the pH of the purifying liquid kept at about 3, and the requirements of upper solid-phase extractor column can be satisfied. The method disclosed by the invention fills up the blank that no method is provided for detecting residual quantity of sodium nitrophenol in aquatic products and other animal foods at present, and has great significance in accurately and scientifically evaluating the quality safety of the aquatic products and making the novel standards of harmful substances in the aquatic products.

Description

technical field [0001] The invention belongs to the technical field of aquatic product detection, and relates to a method for measuring residual sodium nitrophenolate in aquatic products by high performance liquid chromatography-tandem mass spectrometry (LC / APCI-MS / MS). Background technique [0002] The high-efficiency plant growth regulator first discovered by Asahi Chemical Industry Co., Ltd. in Japan in the 1960s is composed of sodium p-nitrophenolate, sodium o-nitrophenolate, and sodium 5-nitro-o-methoxyphenolate. It can It quickly penetrates into plants, regulates and controls the synthesis of nucleic acids, proteins and enzymes in plants, promotes the flow of plant protoplasm, increases cell vitality, and thus promotes germination, rooting, growth and fruiting of plants. Its application in agriculture will inevitably collect in the aquaculture water body with rainwater, etc., resulting in its residue in aquatic products. At the same time, sodium nitrophenolate, as a n...

AI Technical Summary

Problems solved by technology

The accuracy of the TLC-UV method is low, the precision is not ideal, the operation steps are cumbersome, time-consuming and laborious; the high-performance liquid chromatography is detected by an ultraviolet detector, which has more interference and poor sensitivity, and cannot meet the requirements of residue detection.

The physical and chemical properties of sodium nitrophenolate are different from those of nitrophenol. Sodium nitrophenolate is a strong polar compound. It needs to be derivatized to reduce its polarity by gas chromatography before measurement. The operation process is cumbersome.

Sodium o-nitrophenolate has poor sensitivity using conventional liquid chromatography-tandem mass spectrometry with an ESI source

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