CN108680570B - Quality detection method of pseudo-ginseng oral preparation - Google Patents
Quality detection method of pseudo-ginseng oral preparation Download PDFInfo
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Abstract
The invention discloses a quality detection method of a pseudo-ginseng oral preparation, belonging to the technical field of medicine processing detection, which comprises the following specific steps: s1: detecting the content of saponin; s2: detecting the content of pesticide residues; s3: the invention can detect the saponin content, the heavy metal content and the traditional Chinese medicine residual content in the pseudo-ginseng, has simple detection method and accurate detection result, provides quality guarantee for improving the production quality of the pseudo-ginseng oral liquid, can establish a perfect quality detection system of pseudo-ginseng medicinal materials, and provides reliable basis for the processing optimization and quality improvement of pseudo-ginseng preparation.
Description
Technical Field
The invention discloses a quality detection method of a pseudo-ginseng oral preparation, and particularly relates to the technical field of medicine processing detection.
Background
The notoginseng oral liquid has the functions of resisting senility, strengthening body resistance, consolidating constitution, tonifying qi and strengthening heart, strengthening spleen, consolidating constitution, nourishing yin, moistening dryness, promoting the production of body fluid and relieving cough; it also has effects in improving immunity, and increasing leukocyte and hemoglobin. During the preparation process of the pseudo-ginseng oral liquid, the determination of the content of notoginsenoside, the content of heavy metal and the content of pesticide residue is carried out, and a set of complete quality standard of pseudo-ginseng granules is established, so that stable and reliable basis can be provided for the processing optimization of pseudo-ginseng products and the quality of the pseudo-ginseng oral liquid. Therefore, a quality detection method of the pseudo-ginseng oral preparation is put into use to solve the problems.
Disclosure of Invention
The invention aims to provide a quality detection method of a pseudo-ginseng oral preparation, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a quality detection method of a pseudo-ginseng oral preparation comprises the following specific steps:
s1: and (3) detecting the content of the saponin: extracting panax notoginseng saponins from a panax notoginseng oral liquid sample, drying, adding 2-6 mol.L of 15-25 mg of dried total saponins into 50-60% methanol solution-1Hydrolyzing hydrogen chloride at 100-120 ℃ for 5-7 h to completely hydrolyze the panax notoginseng saponins, extracting aglycone with dichloromethane, evaporating to dryness under reduced pressure to obtain 7-9 mg of aglycone, dissolving in 90-95% ethanol to a constant volume of 100-120 ml, and taking the solution as a panax notoginseng saponins sample solution;
adding deionized water into the notoginsenoside sample solution to 150-180 ml, dissolving, passing through macroporous adsorption resin, washing off water-soluble sugar with 80-100 ml of deionized water after column loading is finished, eluting saponin with 200-300 ml of 90-95% ethanol, and keeping for 1-3 ml/min-1Collecting eluent, decompressing and volatilizing, dissolving by using 100-150 ml of 15-30% methanol, passing through cation exchange resin, decompressing and evaporating methanol from the collected methanol elution part, taking 1ml of methanol, measuring the light absorption value after the methanol is developed in a test tube with a plug, and calculating the content of the panax notoginseng saponins according to the average value of 2 times of measurement;
s2: detecting the pesticide residue content: placing 2g of pseudo-ginseng oral liquid into a 100ml conical flask with a plug, adding 20-30 ml of water, soaking overnight, precisely adding 30-40 ml of acetone, weighing, carrying out ultrasonic treatment for 30min, weighing again, supplementing the lost weight with acetone, adding 6-8 g of sodium chloride, precisely adding 20-30 ml of dichloromethane, weighing, carrying out ultrasonic treatment for 15-30 min, weighing again, supplementing the lost weight with dichloromethane, 10000-15000 r.min-1Centrifuging for 5-7 min, quickly transferring the organic phase into a 100ml conical flask with a plug and containing a proper amount of anhydrous sodium sulfate, and standing for 4-6 h;
precisely measuring 35-40 ml, concentrating with 30-50 ℃ water bath under reduced pressure until the mixture is nearly dry, adding a small amount of petroleum ether, repeating the operations until dichloromethane and acetone are removed, dissolving with the petroleum ether, transferring into a 10ml centrifuge tube with a plug scale, adding the petroleum ether to dilute to 5-6 ml, carefully adding 1-2 ml of sulfuric acid, shaking for 1-3 min, and 3000-4000 r.min-1Centrifuging for 10-20 min, taking supernatant, observing the change of a chromatogram on a gas chromatograph, and comparing the chromatogram with a chromatogram of the content of pesticide residues, thereby detecting whether the content of the pesticide residues of the pseudo-ginseng oral liquid reaches the standard or not;
s3: and (3) determination of heavy metal content: weighing 5-7 ml of a pseudo-ginseng oral liquid sample, placing the sample into a digestion tank, adding 8-10 ml of nitric acid, 3-5 ml of hydrofluoric acid and 3-5 ml of hydrogen chloride, carefully shaking to immediately release gas generated, placing the tank at normal temperature for 24-36 h, sealing the tank, placing the tank into a microwave system for digestion, cooling the tank to room temperature, opening the digestion tank in a ventilation environment, filtering the sample into a crucible, placing the crucible on an electric heating plate, heating the crucible to 100-120 ℃ to expel acid, passing the liquid after expelling acid through a 0.4-0.5 mu m filter membrane, diluting the liquid with 2% nitric acid to a constant volume of 25ml, and placing the liquid for later use;
transferring the digestion solution prepared in the process into a colorimetric tube, adding a colorimetric agent, then using deionized water to fix the volume to 25ml to prepare a solution to be detected, using an atomic fluorescence instrument to analyze a sample, and determining the heavy metal content.
Preferably, in step S1, the method for extracting total saponins of panax notoginseng comprises: adding 70% ethanol into Notoginseng radix oral liquid sample at a ratio of 1:12, extracting at high frequency of 50KHZ for 4 times, and performing ultrasonic treatment for 30min each time to obtain Notoginseng radix total saponin with extraction rate of 96.42%.
Preferably, in the step S2, the carrier gas of the gas chromatograph is high-purity nitrogen, and the column flow rate is 1 to 3 ml/min-1Blowing tail gas 50-60 ml/min-1The temperature of a feed inlet is 240-260 ℃, the temperature of a detector is 280-300 ℃, the split ratio of sample injection is 5:1, the temperature programming process is that the initial temperature is 100-120 ℃, the temperature is kept for 1-3 min, and the temperature is 20 ℃ per min-1The temperature is increased to 210-230 ℃ and kept for 1-3 min, and then 10-20 ℃ min-1Heating to 240 ℃ for min-1260Keeping the temperature at 6-8 min.
Preferably, in the step S3, the digestion procedure is to heat up to 160-180 ℃, complete the heating process within 15min, keep for 10-15 min, cool for 5-10 min, and take out.
Preferably, in step S3, the colorimetric agent is a mixture of hydrogen chloride, thiourea and ascorbic acid, wherein the ratio of hydrogen chloride: thiourea: ascorbic acid is 5.5:1.6:0.8, and the addition volume ratio of the color matching agent to the digestion solution is 0.5: 1.
Compared with the prior art, the invention has the beneficial effects that: the method can detect the saponin content, the heavy metal content and the traditional Chinese medicine residual content in the pseudo-ginseng, has simple detection method and accurate detection result, provides quality guarantee for improving the production quality of the pseudo-ginseng oral liquid, can establish a perfect quality detection system of pseudo-ginseng medicinal materials, and improves reliable basis for the processing optimization and the quality of pseudo-ginseng preparation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A quality detection method of a pseudo-ginseng oral preparation comprises the following specific steps:
s1: and (3) detecting the content of the saponin: extracting Notoginseng radix total saponin from Notoginseng radix oral liquid sample, drying, adding 15mg of dried total saponin into 50% methanol solution, and adding 2 mol.L-1Hydrolyzing hydrogen chloride at 100 deg.C for 5 hr to completely hydrolyze Panax notoginsenosides, extracting aglycone with dichloromethane, evaporating to dryness under reduced pressure to obtain aglycone 7mg, dissolving in 90% ethanol to constant volume of 100ml, using high purity nitrogen as carrier gas of gas chromatograph as Panax notoginsenosides sample solution, and column flow rate of 1 ml/min-1Blowing 50 ml/min at the tail-1The temperature of the feed inlet is 240 ℃, the temperature of the detector is 280 DEG CThe sample introduction split ratio is 5:1, the temperature programming process is that the initial temperature is 100 ℃, the temperature is maintained for 1min, and the temperature is 20 ℃ per min-1Heating to 210 deg.C, maintaining for 1min, and heating to 10 deg.C/min-1Heating to 240 ℃ for min-1Keeping at 260 deg.C for 6 min;
adding deionized water into notoginsenoside sample solution to 150ml, dissolving, passing through macroporous adsorbent resin, loading onto column, washing with 80ml deionized water to remove water soluble sugar, eluting with 90% ethanol 200ml to remove saponin, and maintaining for 1 ml/min-1Collecting eluate, evaporating under reduced pressure, dissolving with 100ml and 15% methanol, passing through cation exchange resin, evaporating the methanol from the collected methanol eluate under reduced pressure, collecting 1ml, coloring in test tube with plug, measuring light absorption value, and calculating Notoginseng radix total saponin content according to the average value of 2 times of measurement;
s2: detecting the pesticide residue content: placing 2g of Notoginseng radix oral liquid in 100ml conical flask with plug, adding 20ml of water, soaking overnight, adding 30ml of acetone precisely, weighing, ultrasonic treating for 30min, weighing again, supplementing the lost weight with acetone, adding 6g of sodium chloride, adding 20ml of dichloromethane precisely, weighing, ultrasonic treating for 15min, weighing again, supplementing the lost weight with dichloromethane, 10000 r.min-1Centrifuging for 5min, quickly transferring the organic phase into a 100ml conical flask with a plug and containing a proper amount of anhydrous sodium sulfate, and standing for 4 h; the carrier gas of the gas chromatograph is high-purity nitrogen, and the column flow rate is 1 ml/min-1Blowing 50 ml/min at the tail-1The temperature of the feed inlet is 240 ℃, the temperature of the detector is 280 ℃, the split ratio of the sample injection is 5:1, the temperature programming process is the initial temperature of 100 ℃, the temperature is maintained for 1min, and the temperature is controlled to be 20 ℃ per min-1Heating to 210 deg.C, maintaining for 1min, and heating to 10 deg.C/min-1Heating to 240 ℃ for min-1Keeping at 260 deg.C for 6 min;
precisely measuring 35ml, concentrating with 30 deg.C water bath under reduced pressure to near dryness, adding small amount of petroleum ether until dichloromethane and acetone are removed, dissolving with petroleum ether, transferring into 10ml centrifuge tube with plug scale, adding petroleum ether to dilute to 5ml, carefully adding sulfuric acid 1ml, shaking for 1min, 3000 r.min-1Centrifuging for 10min, collecting supernatant,observing the change of the chromatogram on a gas chromatograph, and comparing the chromatogram with the chromatogram of the pesticide residue content so as to detect whether the pesticide residue content of the pseudo-ginseng oral liquid reaches the standard or not;
s3: and (3) determination of heavy metal content: weighing 5ml of a pseudo-ginseng oral liquid sample, placing the sample into a digestion tank, adding 8ml of nitric acid, 3ml of hydrofluoric acid and 3ml of hydrogen chloride, carefully shaking to immediately release gas generated, placing the tank in a microwave system for digestion after standing at normal temperature for 24 hours, then cooling to room temperature, opening the digestion tank in a ventilation environment, filtering the sample into a crucible, placing the crucible on an electric heating plate, heating to 100 ℃ for acid removal, passing the liquid through a 0.4 mu m filter membrane after acid removal, fixing the volume to 25ml by using 2% dilute nitric acid, and placing the liquid for later use; the digestion procedure is that the temperature is increased to 160 ℃, the temperature increase process is completed within 15min, the temperature is kept for 10min, and the material is taken out after being cooled for 5 min;
transferring the digestion solution prepared in the process into a colorimetric tube, adding a color matching agent, then fixing the volume to 25ml by using deionized water to prepare a solution to be detected, analyzing a sample by using an atomic fluorescence instrument, and determining the heavy metal content of the sample, wherein the color matching agent is a mixture of hydrogen chloride, thiourea and ascorbic acid, wherein the hydrogen chloride: thiourea: ascorbic acid is 5.5:1.6:0.8, and the addition volume ratio of the color matching agent to the digestion solution is 0.5: 1.
Example two
A quality detection method of a pseudo-ginseng oral preparation comprises the following specific steps:
s1: and (3) detecting the content of the saponin: extracting Notoginseng radix total saponin from Notoginseng radix oral liquid sample, drying, adding 25mg of dried total saponin into 60% methanol solution, and adding 6 mol.L-1Hydrolyzing hydrogen chloride at 120 deg.C for 7 hr to completely hydrolyze Panax notoginsenosides, extracting aglycone with dichloromethane, evaporating to dryness under reduced pressure to obtain aglycone 9mg, dissolving in 95% ethanol to constant volume of 120ml, using high purity nitrogen as carrier gas of gas chromatograph as Panax notoginsenosides sample solution, and column flow rate of 3 ml/min-1Blowing 60 ml/min at the tail-1The temperature of the feed inlet is 260 ℃, the temperature of the detector is 300 ℃, the split ratio of the sample injection is 5:1, the temperature programming process is that the initial temperature is 120 ℃, the temperature is maintained for 3min, and the temperature is 20 ℃ per min-1The temperature is increased to 230 ℃ at the speed of (1), and the temperature is kept for 3minThen at 20 ℃ min-1Heating to 240 ℃ for min-1Maintaining at 260 deg.C for 8 min;
adding deionized water into notoginsenoside sample solution to 180ml, dissolving, passing through macroporous adsorbent resin, loading onto column, washing with 100ml deionized water to remove water soluble sugar, eluting with 95% ethanol 300ml to remove saponin, and maintaining for 3 ml/min-1Collecting eluate, evaporating under reduced pressure, dissolving with 150ml and 30% methanol, passing through cation exchange resin, evaporating methanol to dryness under reduced pressure, collecting 1ml, coloring in test tube with plug, measuring light absorption value, and calculating Notoginseng radix total saponin content according to the average value of 2 times;
s2: detecting the pesticide residue content: placing 2g of Notoginseng radix oral liquid in 100ml conical flask with plug, adding water 30ml, soaking overnight, adding acetone 40ml precisely, weighing, ultrasonic treating for 30min, weighing again, supplementing lost weight with acetone, adding sodium chloride 8g, adding dichloromethane 30ml precisely, weighing, ultrasonic treating for 30min, weighing again, supplementing lost weight with dichloromethane, and 15000 r.min-1Centrifuging for 7min, quickly transferring the organic phase into a 100ml conical flask with a plug and containing a proper amount of anhydrous sodium sulfate, and standing for 6 h; the carrier gas of the gas chromatograph is high-purity nitrogen, and the column flow rate is 3 ml/min-1Blowing 60 ml/min at the tail-1The temperature of the feed inlet is 260 ℃, the temperature of the detector is 300 ℃, the split ratio of the sample injection is 5:1, the temperature programming process is that the initial temperature is 120 ℃, the temperature is maintained for 3min, and the temperature is 20 ℃ per min-1The temperature is increased to 230 ℃ at the speed of (1), the temperature is maintained for 3min, and then the temperature is increased to 20 ℃ for min-1Heating to 240 ℃ for min-1Maintaining at 260 deg.C for 8 min;
precisely measuring 40ml, concentrating with 50 deg.C water bath under reduced pressure to near dryness, adding small amount of petroleum ether until dichloromethane and acetone are removed, dissolving with petroleum ether, transferring into 10ml centrifuge tube with plug scale, adding petroleum ether to dilute to 6ml, carefully adding 2ml sulfuric acid, shaking for 3min, 4000 r.min-1Centrifuging for 20min, collecting supernatant, observing chromatogram variation on gas chromatograph, and comparing with chromatogram of pesticide residue content to detect pesticide residue content of Notoginseng radix oral liquidWhether the standard is reached;
s3: and (3) determination of heavy metal content: weighing 7ml of a pseudo-ginseng oral liquid sample, placing the sample into a digestion tank, adding 10ml of nitric acid, 5ml of hydrofluoric acid and 5ml of hydrogen chloride, carefully shaking to immediately release gas generated, placing the tank into a microwave system for digestion after placing for 36 hours at normal temperature, then cooling to room temperature, opening the digestion tank in a ventilation environment, filtering the sample into a crucible, placing the crucible on an electric heating plate, heating to 120 ℃ for acid removal, passing the liquid through a 0.5 mu m filter membrane after acid removal, fixing the volume to 25ml by using 2% dilute nitric acid, and placing for later use; the digestion procedure is that the temperature is increased to 180 ℃, the temperature increase process is completed within 15min, the temperature is kept for 15min, and the digestion solution is taken out after being cooled for 10 min;
transferring the digestion solution prepared in the process into a colorimetric tube, adding a color matching agent, then fixing the volume to 25ml by using deionized water to prepare a solution to be detected, analyzing a sample by using an atomic fluorescence instrument, and determining the heavy metal content of the sample, wherein the color matching agent is a mixture of hydrogen chloride, thiourea and ascorbic acid, wherein the hydrogen chloride: thiourea: ascorbic acid is 5.5:1.6:0.8, and the addition volume ratio of the color matching agent to the digestion solution is 0.5: 1.
EXAMPLE III
A quality detection method of a pseudo-ginseng oral preparation comprises the following specific steps:
s1: and (3) detecting the content of the saponin: extracting Notoginseng radix total saponin from Notoginseng radix oral liquid sample, drying, adding 20mg of dried total saponin into 55% methanol solution, and adding 4 mol.L-1Hydrolyzing hydrogen chloride at 110 deg.C for 6 hr to completely hydrolyze Panax notoginsenosides, extracting aglycone with dichloromethane, evaporating to dryness under reduced pressure to obtain aglycone 8mg, dissolving in 94% ethanol to desired volume of 110ml, using high purity nitrogen as carrier gas of gas chromatograph as Panax notoginsenosides sample solution, and column flow rate of 2 ml/min-1Blowing 55 ml/min at the tail-1The temperature of the feed inlet is 250 ℃, the temperature of the detector is 290 ℃, the split ratio of the sample injection is 5:1, the temperature programming process is that the initial temperature is 110 ℃, the temperature is kept for 2min, and the temperature is 20 ℃ per min-1Heating to 220 deg.C, maintaining for 2min, and heating to 16 deg.C/min-1Heating to 240 ℃ for min-1Keeping at 260 ℃ for 7 min;
dissolving in notoginsenoside sampleAdding deionized water to 160ml, dissolving, passing through macroporous adsorbent resin, loading onto column, washing with 90ml deionized water to remove water soluble sugar, eluting with 93% ethanol 260ml to remove saponin, and maintaining for 2 ml/min-1Collecting eluate, evaporating under reduced pressure, dissolving with 130ml and 25% methanol, passing through cation exchange resin, evaporating the methanol from the collected methanol eluate under reduced pressure, collecting 1ml, coloring in test tube with plug, measuring light absorption value, and calculating Notoginseng radix total saponin content according to the average value of 2 times of measurement;
s2: detecting the pesticide residue content: placing 2g of Notoginseng radix oral liquid in 100ml conical flask with plug, adding 25ml of water, soaking overnight, adding 35ml of acetone, weighing, ultrasonic treating for 30min, weighing again, supplementing the lost weight with acetone, adding 7g of sodium chloride, adding 25ml of dichloromethane, weighing, ultrasonic treating for 20min, weighing again, supplementing the lost weight with dichloromethane, 13000 r.min-1Centrifuging for 6min, quickly transferring the organic phase into a 100ml conical flask with a plug and containing a proper amount of anhydrous sodium sulfate, and standing for 5 h; the carrier gas of the gas chromatograph is high-purity nitrogen, and the column flow rate is 2 ml/min-1Blowing 55 ml/min at the tail-1The temperature of the feed inlet is 250 ℃, the temperature of the detector is 290 ℃, the split ratio of the sample injection is 5:1, the temperature programming process is that the initial temperature is 110 ℃, the temperature is kept for 2min, and the temperature is 20 ℃ per min-1Heating to 220 deg.C, maintaining for 2min, and heating to 15 deg.C/min-1Heating to 240 ℃ for min-1Keeping at 260 ℃ for 7 min;
precisely measuring 38ml, concentrating with 40 deg.C water bath under reduced pressure to near dryness, adding small amount of petroleum ether until dichloromethane and acetone are removed, dissolving with petroleum ether, transferring into 10ml centrifuge tube with plug scale, adding petroleum ether to dilute to 5ml, carefully adding sulfuric acid 1ml, shaking for 2min, 3500 r.min-1Centrifuging for 15min, collecting supernatant, observing chromatogram variation on gas chromatograph, and comparing with chromatogram of pesticide residue content to detect whether pesticide residue content of Notoginseng radix oral liquid reaches standard;
s3: and (3) determination of heavy metal content: weighing 6ml of a pseudo-ginseng oral liquid sample, placing the sample into a digestion tank, adding 9ml of nitric acid, 4ml of hydrofluoric acid and 4ml of hydrogen chloride, carefully shaking to immediately release gas generated, placing the tank in a microwave system for digestion after standing at normal temperature for 30 hours, then cooling to room temperature, opening the digestion tank in a ventilation environment, filtering the sample into a crucible, placing the crucible on an electric heating plate, heating to 110 ℃ for acid removal, passing the liquid through a 0.45 mu m filter membrane after acid removal, fixing the volume to 25ml by using 2% dilute nitric acid, and placing the liquid for later use; the digestion procedure is that the temperature is raised to 170 ℃, the temperature raising process is completed within 15min, the temperature is kept for 14min, and the digestion solution is taken out after being cooled for 8 min;
transferring the digestion solution prepared in the process into a colorimetric tube, adding a color matching agent, then fixing the volume to 25ml by using deionized water to prepare a solution to be detected, analyzing a sample by using an atomic fluorescence instrument, and determining the heavy metal content of the sample, wherein the color matching agent is a mixture of hydrogen chloride, thiourea and ascorbic acid, wherein the hydrogen chloride: thiourea: ascorbic acid is 5.5:1.6:0.8, and the addition volume ratio of the color matching agent to the digestion solution is 0.5: 1.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A quality detection method of a pseudo-ginseng oral preparation is characterized by comprising the following steps: the detection method comprises the following specific steps:
s1: and (3) detecting the content of the saponin: extracting panax notoginseng saponins from a panax notoginseng oral liquid sample, drying, adding 2-6 mol.L of 15-25 mg of dried total saponins into 50-60% methanol solution-1Hydrolyzing hydrogen chloride at 100-120 ℃ for 5-7 h to completely hydrolyze the panax notoginseng saponins, extracting aglycone with dichloromethane, evaporating to dryness under reduced pressure to obtain 7-9 mg of aglycone, dissolving in 90-95% ethanol to a constant volume of 100-120 ml, and taking the solution as a panax notoginseng saponins sample solution;
adding deionized water into the notoginsenoside sample solution to 150-180 ml, dissolving, passing through macroporous adsorbent resin, loading onto column, washing with 80-100 ml deionized water to remove water soluble sugar, and then washing with 90-EEluting saponin with 200-300 ml of 95% ethanol, and keeping for 1-3 ml/min-1Collecting eluent, decompressing and volatilizing, dissolving by using 100-150 ml of 15-30% methanol, passing through cation exchange resin, decompressing and evaporating methanol from the collected methanol elution part, taking 1ml of methanol, measuring the light absorption value after the methanol is developed in a test tube with a plug, and calculating the content of the panax notoginseng saponins according to the average value of 2 times of measurement;
s2: detecting the pesticide residue content: placing 2g of pseudo-ginseng oral liquid into a 100ml conical flask with a plug, adding 20-30 ml of water, soaking overnight, precisely adding 30-40 ml of acetone, weighing, carrying out ultrasonic treatment for 30min, weighing again, supplementing the lost weight with acetone, adding 6-8 g of sodium chloride, precisely adding 20-30 ml of dichloromethane, weighing, carrying out ultrasonic treatment for 15-30 min, weighing again, supplementing the lost weight with dichloromethane, 10000-15000 r.min-1Centrifuging for 5-7 min, quickly transferring the organic phase into a 100ml conical flask with a plug and containing a proper amount of anhydrous sodium sulfate, and standing for 4-6 h;
precisely measuring 35-40 ml, concentrating with 30-50 ℃ water bath under reduced pressure until the mixture is nearly dry, adding a small amount of petroleum ether, repeating the operations until dichloromethane and acetone are removed, dissolving with the petroleum ether, transferring into a 10ml centrifuge tube with a plug scale, adding the petroleum ether to dilute to 5-6 ml, carefully adding 1-2 ml of sulfuric acid, shaking for 1-3 min, and 3000-4000 r.min-1Centrifuging for 10-20 min, taking supernatant, observing the change of a chromatogram on a gas chromatograph, and comparing the chromatogram with a chromatogram of the content of pesticide residues, thereby detecting whether the content of the pesticide residues of the pseudo-ginseng oral liquid reaches the standard or not;
s3: and (3) determination of heavy metal content: weighing 5-7 ml of a pseudo-ginseng oral liquid sample, placing the sample into a digestion tank, adding 8-10 ml of nitric acid, 3-5 ml of hydrofluoric acid and 3-5 ml of hydrogen chloride, carefully shaking to immediately release gas generated, placing the tank at normal temperature for 24-36 h, sealing the tank, placing the tank into a microwave system for digestion, cooling the tank to room temperature, opening the digestion tank in a ventilation environment, filtering the sample into a crucible, placing the crucible on an electric heating plate, heating the crucible to 100-120 ℃ to expel acid, passing the liquid after expelling acid through a 0.4-0.5 mu m filter membrane, diluting the liquid with 2% nitric acid to a constant volume of 25ml, and placing the liquid for later use; in the step S3, the digestion procedure is to heat up to 160-180 ℃, finish the heating process within 15min, keep for 10-15 min, cool for 5-10 min and take out;
transferring the digestion solution prepared in the process into a colorimetric tube, adding a colorimetric agent, then using deionized water to fix the volume to 25ml to prepare a solution to be detected, using an atomic fluorescence instrument to analyze a sample, and determining the heavy metal content.
2. The quality detection method of the panax notoginseng oral preparation according to claim 1, characterized in that: in the step S1, the method for extracting the panax notoginseng saponins comprises the following steps: adding 70% ethanol into Notoginseng radix oral liquid sample at a ratio of 1:12, extracting at high frequency of 50KHZ for 4 times, and performing ultrasonic treatment for 30min each time to obtain Notoginseng radix total saponin with extraction rate of 96.42%.
3. The quality detection method of the panax notoginseng oral preparation according to claim 1, characterized in that: in the step S2, the carrier gas of the gas chromatograph is high-purity nitrogen, and the column flow rate is 1-3 ml/min-1Blowing tail gas 50-60 ml/min-1The temperature of a feed inlet is 240-260 ℃, the temperature of a detector is 280-300 ℃, the split ratio of sample injection is 5:1, the temperature programming process is that the initial temperature is 100-120 ℃, the temperature is kept for 1-3 min, and the temperature is 20 ℃ per min-1The temperature is increased to 210-230 ℃ and kept for 1-3 min, and then 10-20 ℃ min-1Heating to 240 ℃ for min-1Keeping the temperature at 260 ℃ for 6-8 min.
4. The quality detection method of the panax notoginseng oral preparation according to claim 1, characterized in that: in step S3, the colorimetric agent is a mixture of hydrogen chloride, thiourea and ascorbic acid, wherein the ratio of hydrogen chloride: thiourea: ascorbic acid is 5.5:1.6:0.8, and the addition volume ratio of the color matching agent to the digestion solution is 0.5: 1.
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