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A rapid identification method for judging whether Radix Paeoniae Alba has been fumigated with sulfur

A technology of sulfur fumigation and identification method, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of large sampling quantity, weak method specificity, lack of objective basis, etc. Sample processing for simple effects

Inactive Publication Date: 2011-12-21
JIANGSU PROVINCE INST OF TRADITIONAL CHINESE MEDICINE
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AI Technical Summary

Problems solved by technology

[0004] At present, people judge whether the white peony has been fumigated with sulfur, mainly by observing the appearance, color, and tasting the smell, which is highly subjective and lacks objective evidence.
2010 version "Chinese Pharmacopoeia" appendix IXU sulfur dioxide residue determination method adopts titration method to measure, and sensitivity is low, and sample sampling quantity is also larger (10 grams)
It has been reported in the literature that paeoniflorin sulfide in sulfur-fumigated white peony was detected by liquid chromatography-mass spectrometry, but the specificity of the method is not strong when there is no paeoniflorin sulfide as a reference substance

Method used

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  • A rapid identification method for judging whether Radix Paeoniae Alba has been fumigated with sulfur
  • A rapid identification method for judging whether Radix Paeoniae Alba has been fumigated with sulfur
  • A rapid identification method for judging whether Radix Paeoniae Alba has been fumigated with sulfur

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Chromatography system:

[0020] Waters 2695 HPLC-PDA system. Column: Waters Nova-Pak C 18 Column (3.9 x 150 mm, 5 μm). The mobile phase was composed of 0.1% formic acid in water and 0.1% formic acid in methanol. Gradient elution: see Table 1. The elution flow rate was 1.0 mL / min. The temperature of the column oven and the sample chamber were 35°C and 10°C, respectively. The sample injection volume was 20 μL.

[0021] Table 1 Gradient elution table

[0022]

[0023] 2. Mass Spectrometry Conditions

[0024] Waters Micromass Quattro micro mass spectrometer; ESI - Ion source; the spray gas flow rate was set to 400L / h, the temperature was 400°C; the cone airflow was set to 50L / h; the capillary voltage was set to 3500V, the cone voltage of paeoniflorin and its sulfide was set to 25V and 40V respectively, and the collision energy They are respectively set to 15eV and 40eV, and the pressure of the collision gas (argon) is 0.35Pa. The ionic reactions were m / z 449...

Embodiment 2

[0030] 1. Chromatography system

[0031] Waters 2695 HPLC-PDA system. Chromatographic column: Hanbang Hedera ODS-2 (4.6×100mm, 5μm). The mobile phase was composed of 0.2% formic acid in water and 0.2% formic acid in acetonitrile. Gradient elution: see Table 2. The elution flow rate was 1.0 mL / min. The temperature of the column oven and the sample chamber were 35°C and 10°C, respectively. The sample injection volume was 20 μL.

[0032] Table 2 Gradient elution table

[0033]

[0034] 2. Mass Spectrometry Conditions

[0035] Waters Micromass Quattro micro mass spectrometer; ESI - Ion source; the spray gas flow rate was set to 400L / h, the temperature was 400°C; the cone airflow was set to 50L / h; the capillary voltage was set to 3500V, the cone voltage of paeoniflorin and its sulfide was set to 25V and 40V respectively, and the collision energy They are respectively set to 15eV and 40eV, and the pressure of the collision gas (argon) is 0.35Pa. The ionic reactions were ...

Embodiment 3

[0041] 1. Chromatography system

[0042] Waters 2695 HPLC-PDA system. Chromatographic column: Waters Symmetry C8 (2.1×150 mm, 5 μm). The mobile phase consisted of water and methanol. Gradient elution: see Table 3. The elution flow rate was 0.3 mL / min. The temperature of the column oven and the sample chamber were 35°C and 10°C, respectively. The sample injection volume was 20 μL.

[0043] Table 3 Gradient elution table

[0044]

[0045] 2. Mass Spectrometry Conditions

[0046] Waters Micromass Quattro micro mass spectrometer; ESI - Ion source; the spray gas flow rate was set to 400L / h, the temperature was 400°C; the cone airflow was set to 50L / h; the capillary voltage was set to 3500V, the cone voltage of paeoniflorin and its sulfide was set to 25V and 40V respectively, and the collision energy They are respectively set to 15eV and 40eV, and the pressure of the collision gas (argon) is 0.35Pa. The ionic reactions were m / z 449.4 → m / z 327.2 and m / z 543.3 → m / z 259.3...

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Abstract

The invention belongs to the field of authenticity identification of Chinese medicinal materials and decoction pieces, in particular to a method for identifying the quality of Chinese medicinal materials and decoction pieces by using a specific analysis method to detect characteristic chemical components. Illegal acts of sulfur fumigation of Radix Paeoniae Alba occur from time to time, and a rapid identification method is urgently needed. The present invention is based on the conversion of paeoniflorin into paeoniflorin sulfide after sulfur fumigation of Radix Paeoniae Alba, using 50% methanol to ultrasonically extract Radix Paeoniae Alba samples, using reversed-phase liquid chromatography-triple quadrupole mass spectrometry analysis technology for determination, by observing the Radix Paeoniae Alba Whether there are two groups of multi-reaction ion m / z449.4→m / z327.2 and m / z543.3→m / z259.3 chromatographic peaks in sequence in the chromatogram of Paeoniae Alba samples can be used to judge whether Paeoniae Alba is fumigated with sulfur. If there are chromatographic peaks whose reaction ions are m / z543.3→m / z259.3 and m / z449.4→m / z327.2 in the following order, it means that the Radix Paeoniae Alba sample has been fumigated with sulfur. If the chromatographic peak of m / z449.4→m / z327.2 does not appear, and the chromatographic peak of m / z543.3→m / z259.3 does not appear, it can be judged that the white peony root has not been fumigated with sulfur. The invention has the outstanding advantages of small sampling amount (can be as low as 2 mg), high sensitivity, strong specificity, and no need to use paeoniflorin sulfide which is not easily obtained as a reference substance.

Description

【Technical field】 [0001] The invention belongs to the field of authenticity identification of Chinese medicinal materials and decoction pieces, in particular to a method for identifying the quality of Chinese medicinal materials and decoction pieces by using a specific technology to detect characteristic chemical components. 【Background technique】 [0002] Sulfur fumigation, as a traditional method of curing Chinese herbal medicines, has the functions of whitening, pest control, antisepsis and mildew prevention, and is widely used in the processing and storage of Chinese herbal medicines and decoction pieces. However, studies in recent years have found that after sulfur fumigation of Chinese herbal medicines and decoction pieces, toxic sulfur dioxide will remain, and the inherent biological active components will change in quantity or quality, resulting in changes in the quality of medicinal materials and decoction pieces, decreased pharmacological efficacy, and even increase...

Claims

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Application Information

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IPC IPC(8): G01N30/60G01N30/72
Inventor 李松林武洁沈红朱玲英蔡皓贾晓斌
Owner JIANGSU PROVINCE INST OF TRADITIONAL CHINESE MEDICINE
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