CN106093239A - The UPLC/Q TOF MS rapid assay methods of α solanine in a kind of Fructus Lycopersici esculenti - Google Patents

Abstract

The invention discloses the UPLC/Q TOF MS rapid assay methods of α solanine in a kind of Fructus Lycopersici esculenti, belong to food analysis technical field.The methanol solution supersound extraction of ammonium acetate 1% formic acid of the inventive method 1mmol, Oasis HLB solid phase column purifies, through UPLC BEH C18 column (1.7 μm, 50mm × 2.1 mm) chromatographic column separation, use electric spray ion source (ESI) positive ion mode, the α solanine in Fructus Lycopersici esculenti is carried out UPLC/Q TOF MS and analyzes.Present invention 6min analysis time, the range of linearity is 0.01～0.1mg/L；Detection limit 0.5 μ g/kg, quantitative limit 1 μ g/kg.Average recovery rate 70.2%～84.5%, average relative standard's deviation (RSD) is 2.6%～4.2%, has easy and simple to handle, quick, highly sensitive, reproducible, qualitative, quantitative advantage accurately.In the Fructus Lycopersici esculenti of the present invention, the UPLC/Q TOF MS rapid assay methods of α solanine can extract the α solanine of Fructus Lycopersici esculenti more rapid, more fully, to measure the content of α solanine more accurately, significant for improving Fructus Lycopersici esculenti analysis and detection technology and cating quality safety.

Description

The UPLC/Q-TOF-MS rapid assay methods of α-solanine in a kind of Fructus Lycopersici esculenti

Technical field

The present invention relates to the rapid assay methods of a kind of α-solanine, relate more specifically to α-solanine in a kind of Fructus Lycopersici esculenti UPLC/Q-TOF-MS(Ultra Performance Liquid Chromatography-Quadrupole-time of flight mass spectrometry) rapid assay methods, belong to food analysis Detection technique field.

Background technology

Solanine, also known as solanine or solanen or Rhizoma Solani tuber osi toxin, is a kind of steroidal glycoside alkaloid, is mainly seen in Fructus Capsici, eggplant In the plants of Solanaceae such as son, Fructus Lycopersici esculenti, it it is the secondary metabolite of plant.Solanine is not single component, mainly have 6 kinds of alkaloid: α- Solanine, β-solanine, γ-solanine and a small amount of α-chaconine (α-Chaconine), β-chaconine and γ-chaconine.Wherein α- Solanine is main component.It is soluble in hot ethanol, is practically insoluble in ether, chloroform and water.

Solanine has certain toxicity to human body, and edible very small amount is to human body without obvious harm, and 1mg/kg is maximum safety, 1.75mg/kg is then sensitive amount；3-6mg/kg is lethal dose.Morbidity just can be caused into 200mg, 15min to 3h if once eating, as Tongue is numb, nausea and vomiting, stomachache, gastroenteritis, suffer from diarrhoea, vomit, have a fever, the untoward reaction such as dizziness, even result in poisoner god Dead through paralysis, therefore when edible vegetable containing this alkaloid or food it is noted that.

Fructus Lycopersici esculenti is the important vegetable variety that a kind of consumption figure is huge, and in Fructus Lycopersici esculenti, the content of solanine is how much for the safety of Fructus Lycopersici esculenti Edible most important.But the correlation technique of the solanine detection in Fructus Lycopersici esculenti but exists such as to be extracted, detects many problems such as flux, Constrain safe early warning and the quality-monitoring of Fructus Lycopersici esculenti to a certain extent.

The mensuration of the solanine of prior art, the related assays method of the solanine in Fructus Lycopersici esculenti has no report, mainly by change Learn the method for solanine in detection method and determination of immunological methods Rhizoma Solani tuber osi more.Immunological method is mainly Enzyme-linked Immunosorbent Assay Algoscopy；Chemical detection method includes thin layer chromatography, liquid chromatograph, gas chromatogram and LC-MS-MS etc..Existing More in research is liquid chromatograph and liquid chromatograph mass spectrography (LC-MS) technology.High performance liquid chromatography (HPLC) can To realize qualitative and quantitative while solanine, but needing derivative when detecting with HPLC, this is difficult to realize Multicomponent Detect simultaneously.HPLC-UV method pre-treating method is complicated, needs to carry out solid phase column purification.And most common method is LC-MS method Because highly sensitive, selectivity is good, and sample pre-treatments is relatively easy and becomes the main method of solanine detection, such as Chinese patent ZL201210321390.3 discloses α in a kind of Rhizoma Solani tuber osi-solanine and extracts and the method for detection.But LC-MS method exists can not Under conditions of there is no standard solution, screen the defect of more unknown material because in Fructus Lycopersici esculenti containing saccharide, protein, fat, Malic acid, citric acid, vitamin and other impurity and containing acidic materials more, according to patent ZL201210321390.3 Method also cannot extract the response rate in Fructus Lycopersici esculenti α-solanine, and Rhizoma Solani tuber osi and only have 18.6%.

The liquid chromatograph good separating effect that Ultra Performance Liquid Chromatography (UPLC) is relatively common, analyzes speed fast, is especially suitable for Quickly detect in multicomponent.And flight time mass spectrum (TOF-MS) can carry out the accurate mensuration of molecular weight, it is particularly suitable for complexity In substrate, component is the most qualitative, effective analysis method of multicomponent residual during therefore UPLC-TOF-MS becomes complex matrices.

Therefore, in a kind of easy, quick, highly sensitive, reproducible, qualitative, quantitative acid complex matrices Fructus Lycopersici esculenti accurately UPLC/Q-TOF-MS(Ultra Performance Liquid Chromatography-the Quadrupole-time of flight mass spectrometry of α-solanine) rapid assay methods is urgently Develop.

Summary of the invention

It is an object of the invention to provide the UPLC/Q-TOF-MS(Ultra Performance Liquid Chromatography-four of α-solanine in a kind of Fructus Lycopersici esculenti Pole bar flight time tandem mass spectrum) rapid assay methods, simple to operate, quickly and eliminate immune affinity column or solid-phase extraction column Purifying step, not only simplify experiment, and reduces cost.Additionally, the present invention can extract acidity more rapid, more fully Solanine in complex matrices Fructus Lycopersici esculenti, can measure α-solanine content more accurately, has important for improving Fructus Lycopersici esculenti quality safety Meaning.

The technical solution adopted in the present invention is:

The UPLC/Q-TOF-MS rapid assay methods of α-solanine in a kind of Fructus Lycopersici esculenti, is characterized in that comprising the following steps:

(1) in Fructus Lycopersici esculenti, α-solanine extracts: the fresh sample of Fructus Lycopersici esculenti of pretreatment of learning from else's experience, and the methanol solution adding ammonium acetate 1% formic acid extracts Liquid mixes, and carries out supersound process, is repeated 2 times；Merging treatment liquid, sucking filtration, by filtrate rotary distillation to extractum shape, add methanol Extracting solution dissolves, and obtains extracting solution.

(2) purification of α-solanine extracting solution in Fructus Lycopersici esculenti: the most respectively by methanol and water wash Oasis HLB solid phase column (3mL, 60mg), then the extracting solution that step (1) prepares is crossed post, with the chloroform solution drip washing containing methanol, finally use methanol-eluted fractions； Eluent is with vaporized nitrogen to dry, and the residue formic acid containing ammonium acetate-methanol dissolves, standby.

(3) preparation of standard working solution: take α-solanine standard substance, be dissolved to 10.00mL with methanol, takes dense molten respectively Liquid 0.1mL is dissolved to 10.00mL, then crosses after 0.45 μm filter membrane, then takes 1mL and be settled to 10.00mL, take after crossing film 1000 μ L, 100 μ L are settled to 10mL and cross film and obtain the standard solution of 1ppm, 100ppb, then take standard solution 75 μ L, 50 μ taking 1ppm respectively L, 250 μ L, 100 μ L, 10 μ L are settled to 10mL and obtain standard solution 75ppb, 50ppb, 25ppm, 10ppm, 1ppm, treat after crossing film With.

(4) detection of α-solanine in Fructus Lycopersici esculenti: by the standard working solution UPLC/Q-of each Concentraton gradient in step (3) TOF-MS measures the absorption curve of α-solanine mark product of variable concentrations, and with the concentration of α-solanine mark product as abscissa, peak area is Vertical coordinate draws the standard curve of α-solanine mark product；Sample liquid after purifying in step (2) under the same conditions carries out UPLC/ Q-TOF-MS measures, and records the chromatographic peak area of α-solanine in sample liquid, substitutes into standard curve, obtains α-solanine in sample liquid and contain Amount, then obtains α in sample-solanine residual quantity according to the Mass Calculation of sample representated by sample liquid.

Preferably, comprise the following steps:

(1) in Fructus Lycopersici esculenti, α-solanine extracts: take the 10 g fresh sample of Fructus Lycopersici esculenti through pretreatment, adds ammonium acetate 1% first of 10mL1mmol The methanol solution extracting solution mixing of acid, carries out supersound process (55Hz, 30 min), is repeated 2 times；Merging treatment liquid, sucking filtration, will filter Liquid rotary distillation is to extractum shape, and the methanol extract liquid adding 1mL50% dissolves, and obtains extracting solution.

(2) purification of α-solanine extracting solution in Fructus Lycopersici esculenti: the most respectively by 2mL methanol and water wash Oasis HLB solid phase column (3mL, 60mg), then the extracting solution that step (1) prepares is crossed post, with the 1mL chloroform solution drip washing containing 5% methanol, finally use 2mL first Alcohol eluting；Eluent is with vaporized nitrogen to dry, and residue 1mL contains 0.1% formic acid of 1mmol/L ammonium acetate-methanol (30: 70, V/ V) dissolve, standby.

(3) preparation of standard working solution: take 10mg α-solanine standard substance, be dissolved to 10.00mL with methanol, take respectively Concentrated solution 0.1mL is dissolved to 10.00mL, then crosses after 0.45 μm filter membrane, then takes 1mL and be settled to 10.00mL, crosses 0.45 μm filter Take 1000 μ L after film, 100 μ L are settled to 10mL and cross film and obtain the standard solution of 1ppm, 100ppb, then take the mark taking 1ppm respectively Quasi-solution 75 μ L, 50 μ L, 250 μ L, 100 μ L, 10 μ L be settled to 10mL obtain standard solution 75ppb, 50ppb, 25ppm, 10ppm, 1ppm, stand-by after crossing film.

(4) detection of α-solanine in Fructus Lycopersici esculenti: by the standard working solution UPLC/Q-of each Concentraton gradient in step (3) TOF-MS measures the absorption curve of α-solanine mark product of variable concentrations, and with the concentration of α-solanine mark product as abscissa, peak area is Vertical coordinate draws the standard curve of α-solanine mark product；Sample liquid after purifying in step (2) under the same conditions carries out UPLC/ Q-TOF-MS measures, and records the chromatographic peak area of α-solanine in sample liquid, substitutes into standard curve, obtains α-solanine in sample liquid and contain Amount, then obtains α in sample-solanine residual quantity according to the Mass Calculation of sample representated by sample liquid.

Preferably, the testing conditions of described step (4) is:

Chromatographic condition:

Waters UPLC BEH C18 column (1.7 μm, 50mm × 2.1 mm)；Mobile phase A 0.1% formic acid+1 mmol/L Ammonium acetate solution, Mobile phase B is acetonitrile solution；Column temperature: room temperature；Sampling volume: 5 μ L.

Condition of gradient elution is as follows:

Mass Spectrometry Conditions:

Electro-spray ionization pattern: positive ion mode；TOF operational mode: V model；Resolution: 10000～12000；Scanning model Enclose: m/z100～1000；Capillary voltage (Capillary): 3.0kV；Ion source temperature: 120 DEG C；Sample cone voltage (Sample cone): 40V；Extract cone voltage (Extraction cone): 4.0V；Taper hole blowback air flow (Cone): 50L/ h；Desolventizing temperature: 350 DEG C, desolventizing throughput (Desolvation): 800L/h；Tuning solution: leucine enkephalin (m/ Z556.2771), 50pg/ μ L.

Beneficial effects of the present invention:

(1) present invention uses and combines UPLC/Q-TOF-MS based on QuECHERS extracting method and establish the fast of α-solanine in Fructus Lycopersici esculenti Speed assay method, this method is simple to operate, quick and eliminates immune affinity column or solid-phase extraction column purifying step, not only simplifies Experiment, and reduce cost.Achieve the fast qualitative and quantitatively of α-solanine in Fructus Lycopersici esculenti, for improving Fructus Lycopersici esculenti cating quality Safety is significant.

(2) due to Fructus Lycopersici esculenti sample itself, containing saccharide, protein, fat, malic acid, citric acid, vitamin and other is miscellaneous Matter and containing acidic materials more, the present invention use simultaneously mixed solvent extract and solid phase extraction method process sample.Use The methanol solution supersound extraction of ammonium acetate 1% formic acid of 1mmol, Oasis HLB solid phase column purifies, processes sample, interference Background is minimum, and the response rate is high.

(3) using the 0.1% formic acid-methanol solution of 1mmol/L ammonium acetate as flowing phase, α-solanine can obtain very Good separation, retention time is: α-solanine 4.06min, and this method detection time 6min, detection speed is fast.

(4) α-solanine content during the present invention uses UPLC/Q-TOF-MS legal quantitative determination Fructus Lycopersici esculenti, adding of α-solanine The mark response rate is between 70.2%～85.4%, and average relative standard's deviation (RSD) is between 2.6%～4.2%, detection limit of the present invention 0.5 μ g/kg, quantitative limit 1 μ gkg, highly sensitive, reproducible, for ensureing that our people's food safety and export abroad trade are good for Kang Fazhan provides strong technical support.

(5) UPLC/Q-TOF-MS can extract accurate quasi-molecular ion quality using as quantitatively needs, the most permissible Get rid of the interference of similar mass number quasi-molecular ions, thus only carry out first mass spectrometric scanning and i.e. can get good chromatographic peak, make quantitatively Method is greatly simplified.

Accompanying drawing explanation

Accompanying drawing 1 is standard curve；

Accompanying drawing 2 is α in reference substance-solanine mass spectrum；

Accompanying drawing 3 is α in Fructus Lycopersici esculenti-solanine mass spectrum；

Accompanying drawing 4 is the selection ion flow graph of α-solanine in Fructus Lycopersici esculenti；

Accompanying drawing 5 is the selection ion flow graph of positive Fructus Lycopersici esculenti sample.

Detailed description of the invention

In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but the present invention Content is not limited solely to the following examples, and embodiment is not construed as limiting the scope of the present invention.

The instrument used in embodiment:

ACQUITY Ultra Performance LC Ultra Performance Liquid Chromatography, Thermo hypersll gold C18 chromatographic column (2.1 × 100mm, 1.9 m), Waters Xevo Q-ToF level Four bar branch's time mass spectrum instrument (Waters, US)； T25BS2 type high speed dispersion refiner (IKA company of Germany), 3K30 type high speed centrifuge (Sigma Co., USA)；Laborota 4000 type Rotary Evaporators (Heidolph company of Germany)；AE-240 type electronic balance (Mettler-Toledo company of Switzerland).

Medicine and standard substance: α-solanine standard substance (purity > 99%, Sigma Co., USA provides)；Methanol (chromatographically pure, moral Meck company of state), formic acid (chromatographically pure, Sigma Co., USA)；Experimental water is deionized water.Ammonium acetate (chromatographically pure, the U.S. Sigma company)；Acetonitrile (chromatographically pure, Sai Mo flies generation department of pediatrics skill (Chinese) company limited).(Waters is public for Oasis HLB solid phase column Department, 3mL, 60mg).

Sample: commercially available Lycopersicon esculentum and little Fructus Lycopersici esculenti.

Embodiment: the UPLC/Q-TOF-MS rapid assay methods of α-solanine in Fructus Lycopersici esculenti:

The little Fructus Lycopersici esculenti of yellow, maturation after it is red little Fructus Lycopersici esculenti, maturation after to be green little Fructus Lycopersici esculenti, one-tenth by being after the maturation of collection It is after the normal Fructus Lycopersici esculenti of yellow and maturation to be that red five kinds of Fructus Lycopersici esculenti samples of normal Fructus Lycopersici esculenti are divided into according to ripe and immaturity after ripe Two groups of totally ten samples, often group sample is according to quartering division to 500g, this sample is divided into 2 × 200g two parts, adds with food Work machine is pulverized, to be measured in-20 DEG C of airtight preservations of refrigerator-freezer.

To operate the most in accordance with the following steps through pretreated two groups ten Fructus Lycopersici esculenti samples to be measured:

(1) in Fructus Lycopersici esculenti, α-solanine extracts: take the 10 g fresh sample of Fructus Lycopersici esculenti through pretreatment, adds ammonium acetate 1% first of 10mL1mmol The methanol solution extracting solution mixing of acid, carries out supersound process (55Hz, 30 min), is repeated 2 times；Merging treatment liquid, sucking filtration, will filter Liquid rotary distillation is to extractum shape, and the methanol extract liquid adding 1mL50% dissolves, and obtains extracting solution.

(2) purification of α-solanine extracting solution in Fructus Lycopersici esculenti: the most respectively by 2mL methanol and water wash Oasis HLB solid phase column (3mL, 60mg), then the extracting solution that step (1) prepares is crossed post, with the 1mL chloroform solution drip washing containing 5% methanol, finally use 2mL first Alcohol eluting；Eluent is with vaporized nitrogen to dry, and residue 1mL contains 0.1% formic acid of 1mmol/L ammonium acetate-methanol (30: 70, V/ V) dissolve, standby.

(3) preparation of standard working solution: take 10 mg α-solanine standard substance, be dissolved to 10.00mL with methanol, respectively Take concentrated solution 0.1mL and be dissolved to 10.00 mL, after then crossing 0.45 μm filter membrane, then take 1mL and be settled to 10.00mL, cross 0.45 μm Take 1000 μ L after filter membrane, 100 μ L are settled to 10mL and cross film and obtain the standard solution of 1ppm, 100ppb, then take and take 1ppm's respectively Standard solution 75 μ L, 50 μ L 250 μ L, 100 μ L, 10 μ L be settled to 10mL obtain standard solution 75ppb, 50ppb, 25ppm, 10ppm, 1ppm, stand-by after crossing film.

(4) detection of α-solanine in Fructus Lycopersici esculenti: by the standard working solution UPLC/Q-of each Concentraton gradient in step (3) TOF-MS measures the absorption curve of α-solanine mark product of variable concentrations, and with the concentration of α-solanine mark product as abscissa, peak area is Vertical coordinate draws the standard curve of α-solanine mark product；Sample liquid after purifying in step (2) under the same conditions carries out UPLC/ Q-TOF-MS measures, and records the chromatographic peak area of α-solanine in sample liquid, substitutes into standard curve, obtains α-solanine in sample liquid and contain Amount, then obtains α in sample-solanine residual quantity according to the Mass Calculation of sample representated by sample liquid.

The testing conditions of described step (4) is:

Chromatographic condition:

Waters UPLC BEH C18 column (1.7 μm, 50mm × 2.1 mm)；Mobile phase A 0.1% formic acid+1 mmol/L Ammonium acetate solution, Mobile phase B is acetonitrile solution；Column temperature: room temperature；Sampling volume: 5 μ L.

Condition of gradient elution is shown in Table 1:

Table 1: the gradient elution program of embodiment 1

Mass Spectrometry Conditions:

Electro-spray ionization pattern: positive ion mode；TOF operational mode: V model；Resolution: 10000～12000；Scanning Scope: m/z100～1000；Capillary voltage (Capillary): 3.0kV；Ion source temperature: 120 DEG C；Sample cone voltage (Sample cone): 40V；Extract cone voltage (Extraction cone): 4.0V；Taper hole blowback air flow (Cone): 50L/ h；Desolventizing temperature: 350 DEG C, desolventizing throughput (Desolvation): 800L/h；Tuning solution: leucine enkephalin (m/ Z556.2771), 50pg/ μ L.

With the chromatographic peak area of standard working solution, its respective concentration is carried out regression analysis, obtain standard working curve and be shown in Table 2。

The standard curve of α-solanine in table 2 Fructus Lycopersici esculenti bare substrate

Recovery of standard addition and repeatability:

0.01mg/kg, 0.05mg/kg and the pitch-based sphere of 0.1 3 concentration of mg/kg is added in the Fructus Lycopersici esculenti without α-solanine, The determination of residual amount is carried out by above-mentioned process step.Mensuration concentration and pesticide theory are added concentration compare, obtain pesticide and add Adding the response rate, each pitch-based sphere parallel assay 6 times, obtain its relative standard deviation, measurement result is shown in Table 3.Can be seen by table 3 Going out, in 3 mark-on levels, the average recovery rate of α-solanine is 70.2%～84.5%, and average relative standard's deviation (RSD) is 2.6%～4.2%, illustrate that the response rate of the inventive method is higher, reproducible.

The response rate of α-solanine and repeatability (n=6) in table 3 embodiment 1

Detection limit: the α of variable concentrations-solanine extraction standard working solution is injected instrument, with 3 times of noises of quota ion chromatographic peak Be detection limit (LOD) than corresponding toxin least concentration, detection limit be 0.5 μ g/kg (S/N >=3)；With 10 times of noises Being quantitative detection limit (LOQ) than corresponding toxin least concentration, quantitative detection limit is 1 μ g/kg (S/N >=10).

In ten Fructus Lycopersici esculenti samples, the content of α-solanine is shown in Table 4 after testing:

The content of the α-solanine in different Fructus Lycopersici esculenties in table 4 embodiment:

As seen from Table 4, ripe Fructus Lycopersici esculenti does not contains α-solanine, and containing α-eggplant in the immaturity Fructus Lycopersici esculenti sample of different cultivars Alkali, although content is relatively low, but utilize the inventive method can accurately record the α in immaturity Fructus Lycopersici esculenti-solanine content.

Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or Change among still in the protection domain of the invention.

Claims (6)

1. a UPLC/Q-TOF-MS rapid assay methods for α-solanine in Fructus Lycopersici esculenti, is characterized in that, comprise the following steps:

1) in Fructus Lycopersici esculenti, α-solanine extracts: the fresh sample of Fructus Lycopersici esculenti of pretreatment of learning from else's experience, and the methanol solution adding ammonium acetate 1% formic acid extracts Liquid mixes, and carries out supersound process, is repeated 2 times；Merging treatment liquid, sucking filtration, by filtrate rotary distillation to extractum shape, add methanol Extracting solution dissolves, and obtains extracting solution；

2) purification of α-solanine extracting solution in Fructus Lycopersici esculenti: the most respectively with methanol and water wash Oasis HLB solid phase column (3mL, 60mg), then by step 1) extracting solution prepared crosses post, with the chloroform solution drip washing containing methanol, finally uses methanol-eluted fractions；Eluent is used Vaporized nitrogen is to dry, and the residue formic acid containing ammonium acetate-methanol dissolves, standby；

3) preparation of standard working solution: take α-solanine standard substance, be dissolved to 10.00mL with methanol, take concentrated solution respectively 0.1mL is dissolved to 10.00mL, then crosses after 0.45 μm filter membrane, then takes 1mL and be settled to 10.00mL, take after crossing film 1000 μ L, 100 μ L is settled to 10mL and crosses film and obtain the standard solution of 1ppm, 100ppb, then take take respectively the standard solution 75 μ L of 1ppm, 50 μ L, 250 μ L, 100 μ L, 10 μ L are settled to 10mL and obtain standard solution 75ppb, 50ppb, 25ppm, 10ppm, 1ppm, treat after crossing film With；

4) detection of α-solanine in Fructus Lycopersici esculenti: by step 3) in the standard working solution UPLC/Q-TOF-MS of each Concentraton gradient Measuring the absorption curve of α-solanine mark product of variable concentrations, with the concentration of α-solanine mark product as abscissa, peak area is vertical coordinate Draw the standard curve of α-solanine mark product；Under the same conditions by step 2) in purify after sample liquid carry out UPLC/Q-TOF- MS measures, and records the chromatographic peak area of α-solanine in sample liquid, substitutes into standard curve, obtains α in sample liquid-solanine content, so α in sample-solanine residual quantity is obtained afterwards according to the Mass Calculation of sample representated by sample liquid.

The UPLC/Q-TOF-MS rapid assay methods of α-solanine, its feature in a kind of Fructus Lycopersici esculenti the most according to claim 1 Be, described step 4) in chromatographic condition be: Waters UPLC BEH C18 column (1.7 μm, 50mm × 2.1 mm)；Stream Dynamic phase A is 0.1% formic acid+1mmol/L ammonium acetate solution, and Mobile phase B is acetonitrile solution；Column temperature: room temperature；Sampling volume: 5 μ L.

The UPLC/Q-TOF-MS rapid assay methods of α-solanine, its feature in a kind of Fructus Lycopersici esculenti the most according to claim 1 It is that the elution requirement of described eluting is:

。

The UPLC/Q-TOF-MS rapid assay methods of α-solanine, its feature in a kind of Fructus Lycopersici esculenti the most according to claim 1 Be, described step 4) in Mass Spectrometry Conditions be: electro-spray ionization pattern: positive ion mode；TOF operational mode: V model；Differentiate Rate: 10000～12000；Sweep limits: m/z100～1000；Capillary voltage (Capillary): 3.0kV；Ion source temperature: 120 ℃；Sample cone voltage (Sample cone): 40V；Extract cone voltage (Extraction cone): 4.0V；Taper hole blowback Throughput (Cone): 50L/h；Desolventizing temperature: 350 DEG C, desolventizing throughput (Desolvation): 800 L/h；Tune molten Liquid: leucine enkephalin (m/z556.2771), 50pg/ μ L.

The UPLC/Q-TOF-MS rapid assay methods of α-solanine, its feature in a kind of Fructus Lycopersici esculenti the most according to claim 1 Be, described step 4) in the regression equation that obtains be Area=1148.97 × Amt+34.1348；r=0.9999；Wherein, Area is Peak area；Amt is sample concentration after constant volume.

6. according to the UPLC/Q-TOF-MS quickly side of mensuration of α-solanine in a kind of Fructus Lycopersici esculenti described in claim 1-5 any one Method, is characterized in that, comprises the following steps:

1) in Fructus Lycopersici esculenti, α-solanine extracts: takes the 10 g fresh sample of Fructus Lycopersici esculenti through pretreatment, adds the ammonium acetate 1% of 10 mL 1mmol The methanol solution extracting solution mixing of formic acid, carries out supersound process (55Hz, 30 min), is repeated 2 times；Merging treatment liquid, sucking filtration, will Filtrate rotary distillation is to extractum shape, and the methanol extract liquid adding 1mL50% dissolves, and obtains extracting solution；

2) purification of α-solanine extracting solution in Fructus Lycopersici esculenti: the most respectively with 2mL methanol and water wash Oasis HLB solid phase column (3mL, 60mg), then by step 1) extracting solution prepared crosses post, with the 1mL chloroform solution drip washing containing 5% methanol, finally washes with 2mL methanol De-；Eluent is with vaporized nitrogen to dry, and 0.1% formic acid-methanol (30: 70, V/V) that residue contains 1mmol/L ammonium acetate with 1mL is molten Solve, standby；

3) preparation of standard working solution: take 10 mg α-solanine standard substance, be dissolved to 10.00mL with methanol, take dense molten respectively Liquid 0.1mL is dissolved to 10.00mL, then crosses after 0.45 μm filter membrane, then takes 1mL and be settled to 10.00mL, take after crossing film 1000 μ L, 100 μ L are settled to 10mL and cross film and obtain the standard solution of 1ppm, 100ppb, then take standard solution 75 μ L, 50 μ taking 1ppm respectively L, 250 μ L, 100 μ L, 10 μ L are settled to 10mL and obtain standard solution 75ppb, 50ppb, 25ppm, 10ppm, 1ppm, treat after crossing film With；

4) detection of α-solanine in Fructus Lycopersici esculenti: by step 3) in the standard working solution UPLC/Q-TOF-MS of each Concentraton gradient Measuring the absorption curve of α-solanine mark product of variable concentrations, with the concentration of α-solanine mark product as abscissa, peak area is vertical coordinate Draw the standard curve of α-solanine mark product；Under the same conditions by step 2) in purify after sample liquid carry out UPLC/Q-TOF- MS measures, and records the chromatographic peak area of α-solanine in sample liquid, substitutes into standard curve, obtains α in sample liquid-solanine content, so α in sample-solanine residual quantity is obtained afterwards according to the Mass Calculation of sample representated by sample liquid.