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Screening method of illegal additives in seal and ginseng capsules

A technology of illegally adding ginseng, applied in the field of detection and analysis, can solve the problems of large interference, poor accuracy and reliability, and achieve the effects of good accuracy and reliability, efficient extraction, and reduced matrix interference

Inactive Publication Date: 2019-11-19
GUANGDONG PHARMA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defects that the screening of illegal additives in sea dog ginseng pills by existing fingerprint technology is limited to the extraction of a limited class of medicinal ingredients or a small amount of ingredients, large interference, poor accuracy and reliability or insufficient, provide a screening method for illegal additives in sea dog ginseng pills

Method used

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  • Screening method of illegal additives in seal and ginseng capsules
  • Screening method of illegal additives in seal and ginseng capsules
  • Screening method of illegal additives in seal and ginseng capsules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Example 1 Optimization of salting out and phase separation extraction conditions

[0061] This embodiment provides a screening method, which is specifically as follows:

[0062] 11 batches of Seagou Ginseng Pills were purchased through physical stores and online channels. For detailed information of the samples, see Table 1. Accurately weigh 0.1g of the crushed sample powder into a closed microwave extraction tank, add a certain amount of organic solvent and water respectively, shake to make it fully miscible, extract at 70℃ for 10 minutes, cool to room temperature and add a certain amount of inorganic salt , Shake, transfer it to a 50mL centrifuge tube after it is completely dissolved, centrifuge at 3500rpm / min for 5min, take the organic phase and blow dry with nitrogen, dissolve an appropriate amount of methanol and filter with a 0.22μm filter membrane for HPLC analysis.

[0063] The HPLC analysis process is as follows: The selected chromatographic column is YMC-Triart C18 ...

Embodiment 2

[0087] Example 2 Establishment of a multi-level fingerprint database of Haigou ginseng pills

[0088] This embodiment provides the establishment of a multi-level fingerprint database of Haigou Ginseng Pills, which specifically includes ultraviolet spectrum detection and fluorescence spectrum detection.

[0089] The process of UV spectrum detection is as follows: DAD detector records the chromatogram, and uses Chemstation software to process the collected data.

[0090] The process of fluorescence spectrum detection is as follows: The detection signal in the FLD detector is detected at an excitation wavelength of 280 or 275 nm and an emission wavelength of 330 or 470 nm, respectively.

[0091] (1) Spectral characteristics of Seal Ginseng Pills

[0092] The study on the spectral characteristics of Seagou Ginseng Pills and 16 kinds of illegal additives found that the samples of Seagou Ginseng Pills and illegal additives obtained at the detection wavelength of 220nm have the most informatio...

Embodiment 3

[0107] Example 3 Application of Sea Gou Ginseng Pill Multi-level Atlas

[0108] Using the multi-level map screening method for the seagou ginseng pill provided in Example 2 (4), 5 samples on the market were screened, and the results are shown in Figure 14 . by Figure 14 (a) It can be clearly seen that in the HPLC-UV fingerprint of the unknown sample, except for SS3, which has several unknown peaks, the remaining four are basically consistent with R0; Figure 14 (b) shows the possible presence of testosterone in SS5, the secondary fingerprint ( Figure 14 (c)) Its existence is further confirmed, and the results of spectral matching are shown in Table 3. It can be seen from Table 3 that the spectral matching degree of testosterone is higher than 950, so it can be confirmed that testosterone exists in sample 5. The test results were verified by three parallel experiments, and the content calculation results showed that the content of testosterone was 20.5μg / g, and the RSD was ...

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Abstract

The invention relates to a screening method of illegal additives in seal and ginseng capsules. The screening method comprises the following steps: adding organic solvent and water in seal and ginsengcapsule powder sample, performing microwave-assisted extraction, and then adding salting-out agent, shaking and vibrating, centrifuging and splitting phase, taking the upper phase to dry, performing HPLC analysis after dissolving and filtering, and then comparing with the seal and ginseng capsule multi-dimensional fingerprint spectrum and the chromatographic information of the illegal additives, and analyzing the same. The method of utilizing microwave assistance, salting-out, phase-splitting, extraction, and multi-dimensional fingerprint spectrum combination is used for screening the illegaladditives in the seal and ginseng capsules; an optimal extraction condition is determined by optimizing each composition element; the chromatographic behavior is researched according to the spectrum characteristics of the illegal additives; and the multi-dimensional fingerprint characteristics of the seal and ginseng capsules are acquired by combining the chromatographic information of multiple batches of seal and ginseng capsules. The screening method disclosed by the invention can detect 16 illegal additives, the screening efficiency is high, and excellent accuracy and reliability are provided.

Description

Technical field [0001] The invention belongs to the technical field of detection and analysis, and specifically relates to a screening method for illegal additives in seagou ginseng pills. Background technique [0002] Sea Dog Ginseng Pills (FSGP) is a kind of aphrodisiac health care product. Its active ingredients include wolfberry, ginseng, yam, cinnamon, epimedium and eucommia and other traditional Chinese medicines in addition to sea dog powder. It has obvious effects on sexual dysfunction. effect. At present, there are many brands of Seagou Ginseng Pills on the market, and the quality is uneven. There are illegal additions of chemical drugs to enhance the efficacy. Long-term use of health products containing these illegal additives may cause hypotension, shock, stroke, etc. Serious adverse drug reactions. Common illegal additives include phosphodiesterase type 5 (PDE-5) inhibitors, male hormones, alpha receptor antagonists, and plant extracts. New illegal additives are sti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88G01N2030/027G01N2030/047G01N2030/062G01N2030/065G01N2030/884
Inventor 范华均张薇王珂
Owner GUANGDONG PHARMA UNIV
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