CN-122017086-A - Chromatographic mass spectrometry/mass spectrometry rapid detection method for heliotropin in essential oil for cleaning

CN122017086ACN 122017086 ACN122017086 ACN 122017086ACN-122017086-A

Abstract

The invention provides a chromatographic mass spectrometry/mass spectrometry rapid detection method of heliotropin in essential oil for cleaning. The chromatographic mass spectrometry/mass spectrometry rapid detection method of the heliotropin in the essential oil for cleaning comprises the following steps of S1, sample pretreatment, ultrasonic extraction of the essential oil sample by using a mixed solvent of normal hexane and ethyl acetate to obtain an extracting solution, purification of the extracting solution by a silica gel solid-phase extraction column, elution by normal hexane, elution by ethyl acetate and eluent collection, S2, gas chromatography-tandem mass spectrometry analysis, wherein the eluent obtained in the S1 is subjected to GC-MS/MS analysis, the chromatographic column is a weak-polarity or nonpolar capillary column, and qualitative and quantitative detection of the heliotropin is carried out by an internal standard method by adopting a multi-reaction monitoring mode. The chromatographic mass spectrometry/mass spectrometry rapid detection method of heliotropin in the essential oil for cleaning provided by the invention has the advantages of simple and convenient processing steps, good sensitivity, high accuracy and shorter analysis duration.

Inventors

LI CHUNYAN
ZHANG ZIHAO
Mai Xiaoxia
HUO WEIJIANG
TAN ZHIYI
XIAO QIAN

Assignees

广州海关技术中心

Dates

Publication Date: 20260512
Application Date: 20260331

Claims (8)

1. The method for rapidly detecting the chromatographic mass spectrum/mass spectrum of the heliotropin in the essential oil for cleaning is characterized by comprising the following steps of: s1, sample pretreatment, namely performing ultrasonic extraction on an essential oil sample by using a mixed solvent of normal hexane and ethyl acetate to obtain an extracting solution, purifying the extracting solution by a silica gel solid phase extraction column, eluting by using normal hexane, eluting by using ethyl acetate, and collecting an eluent; s2, performing gas chromatography-tandem mass spectrometry, namely performing GC-MS/MS analysis on the eluent obtained in the step S1, wherein a chromatographic column is a weak-polarity or nonpolar capillary column, and performing qualitative and quantitative detection on heliotropin by an internal standard method by adopting a multi-reaction monitoring mode.
2. The method for rapid detection of the chromatograph mass spectrum/mass spectrum of heliotropin in the essential oil for cleaning according to claim 1, wherein in the step S1, the volume ratio of n-hexane to ethyl acetate is 5:1.
3. The rapid chromatographic mass spectrometry/mass spectrometry detection method for heliotropin in essential oil for cleaning according to claim 1, wherein in the step S1, the silica gel solid phase extraction column is a RIPP silica gel solid phase extraction column.
4. The rapid chromatographic mass spectrometry/mass spectrometry detection method of heliotropin in essential oil for cleaning according to claim 1, wherein in S1, the volume of n-hexane used for the leaching is 2 mL, and the volume of ethyl acetate used for the eluting is 2 mL.
5. The method for rapidly detecting the chromatographic mass spectrum/mass spectrum of the heliotropin in the essential oil for cleaning according to claim 1, wherein in the step S2, the gas chromatography condition is that the temperature of a sample inlet is 280 ℃, the carrier gas is helium, the flow rate is 3 mL/min, the split sample is fed in a split ratio of 5:1, and the temperature programming condition is that the initial temperature is kept at 2 min at 40 ℃ and the temperature is raised to 290 ℃ at a rate of 10 ℃/min and kept at 6 min.
6. The method for rapidly detecting the chromatograph mass spectrum/mass spectrum of the heliotropin in the essential oil for cleaning according to claim 1, wherein in the step S2, the mass spectrum condition is an EI ion source, ionization energy is 70 eV, ion source temperature is 230 ℃, and quadrupole temperature is 150 ℃.
7. The method for rapidly detecting the chromatograph mass spectrum/mass spectrum of the heliotropin in the essential oil for cleaning according to claim 1, wherein in the step S2, the monitoring ion pairs in the multi-reaction monitoring mode are heliotropin, parent ion m/z 150, child ion m/z 122, m/z 65 and m/z 39, wherein m/z 150>122 is a quantitative ion pair, the internal standard is benzaldehyde, and the monitoring ion pairs are parent ion m/z 106, child ion m/z 77 and m/z 51.
8. The method for rapid detection of the chromatograph mass spectrum/mass spectrum of heliotropin in essential oil for cleaning according to claim 1, wherein the internal standard adopted by the internal standard method is benzaldehyde.

Description

Chromatographic mass spectrometry/mass spectrometry rapid detection method for heliotropin in essential oil for cleaning Technical Field The invention relates to the technical field of analytical chemistry, in particular to a chromatographic mass spectrometry/mass spectrometry rapid detection method of heliotropin in essential oil for cleaning. Background Heliotropin is a synthetic perfume having a mirabilis jalapa fragrance, and is widely used as a fragrance composition and a fragrance fixative. Meanwhile, the novel drug can be used for synthesizing novel drugs, is listed as a first type of easy-to-prepare chemical, and is listed in the export control list of dual-purpose items of the people's republic of China, and the production, the sales and the import and export of the novel drug are strictly controlled and need to be effectively monitored. Currently, methods for detecting heliotropin include Gas Chromatography (GC), high Performance Liquid Chromatography (HPLC), and infrared spectroscopy. However, when the gas chromatography is aimed at a complex essential oil matrix, the misjudgment risk exists qualitatively, the quantitative analysis of the area normalization method is seriously interfered by the matrix and has poor reproducibility, the high-performance liquid chromatography has high pretreatment requirements, the separation effect of micro-components in the complex matrix is limited, and the infrared spectrum rule cannot accurately quantify. Therefore, it is necessary to provide a new chromatographic mass spectrometry/mass spectrometry rapid detection method for heliotropin in essential oil for cleaning, which solves the above technical problems. Disclosure of Invention The invention solves the technical problem of providing the chromatographic mass spectrometry/mass spectrometry rapid detection method for the heliotropin in the essential oil for cleaning, which has the advantages of simple processing steps, good sensitivity, high accuracy and short analysis duration. In order to solve the technical problems, the chromatographic mass spectrometry/mass spectrometry rapid detection method of heliotropin in the essential oil for cleaning provided by the invention comprises the following steps: s1, sample pretreatment, namely performing ultrasonic extraction on an essential oil sample by using a mixed solvent of normal hexane and ethyl acetate to obtain an extracting solution, purifying the extracting solution by a silica gel solid phase extraction column, eluting by using normal hexane, eluting by using ethyl acetate, and collecting an eluent; s2, performing gas chromatography-tandem mass spectrometry, namely performing GC-MS/MS analysis on the eluent obtained in the step S1, wherein a chromatographic column is a weak-polarity or nonpolar capillary column, and performing qualitative and quantitative detection on heliotropin by an internal standard method by adopting a multi-reaction monitoring mode. Preferably, in S1, the volume ratio of n-hexane to ethyl acetate is 5:1. Preferably, in the step S1, the silica gel solid phase extraction column is a RIPP silica gel solid phase extraction column. Preferably, in S1, the volume of n-hexane used for the elution is 2 mL, and the volume of ethyl acetate used for the elution is 2 mL. Preferably, in the step S2, the gas chromatography is carried out under the conditions that the temperature of a sample inlet is 280 ℃, the carrier gas is helium, the flow rate is 3 mL/min, the split sample injection is carried out, the split ratio is 5:1, the temperature programming is carried out under the conditions that the initial temperature is kept at 40 ℃ to be 2 min, and the temperature is raised to 290 ℃ at the rate of 10 ℃/min to be 6 min. Preferably, in the step S2, the mass spectrum condition is EI ion source, ionization energy 70 eV, ion source temperature 230 ℃ and quadrupole temperature 150 ℃. Preferably, in the step S2, the monitoring ion pair in the multi-reaction monitoring mode is heliotropin, parent ion m/z 150, ion m/z 122, m/z 65 and m/z 39, wherein m/z 150>122 is a quantitative ion pair, the internal standard is benzaldehyde, and the monitoring ion pair is parent ion m/z 106, child ion m/z 77 and m/z 51. Preferably, the internal standard used in the internal standard method is benzaldehyde. Compared with the related art, the chromatographic mass spectrometry/mass spectrometry rapid detection method for the heliotropin in the essential oil for cleaning has the following beneficial effects: The invention provides a chromatographic mass spectrometry/mass spectrometry rapid detection method of heliotropin in essential oil for cleaning, which is characterized in that the heliotropin in essence is extracted by ethyl acetate through ultrasonic, purification and elution are carried out by a silica gel solid phase extraction column, and the determination is carried out by a gas chromatography-tandem mass spectrometry MRM mode. The result shows that the method has t