CN106153773B - Utilize the method for l-carnitine in ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder - Google Patents
Utilize the method for l-carnitine in ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses a kind of methods using l-carnitine in ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder, it is separated using CORTECS HILIC chromatographic column, using -0.1% formic acid solution of methanol as mobile phase, 25 DEG C of column temperature, sample volume 2 μ L, flow velocity 0.3ml/min, mass ion source is electric spray ion source, cation scan pattern, scanning mode are multiple-reaction monitoring, and quota ion is m/z 162.2 → 103.1.Method of the invention is easy to operate, high sensitivity, reproducible, the measurement for the l-carnitine that can be used in baby formula milk powder.
Description
Technical field
The present invention relates to Food Inspection technical field, the fast quantification of l-carnitine in especially a kind of baby formula milk powder
The method of inspection.
Background technique
L-carnitine (L-Carnitine), the entitled 3- carboxyl -4-N- trimethyl-aminobutyric acid (3-Hydroxy-4-N- of chemistry
Trimethyla minobutyrate), it is a kind of amino acid being widely present in human body, is mainly distributed on muscle, heart
In, major function is that transhipment fat enters mitochondria, promotes burning fatty acid, provides energy for body[1-3], people can not only lead to
It crosses food and obtains l-carnitine, and can voluntarily synthesize in vivo[4], but infant itself synthesis capability is lower, it is therefore necessary in baby children
It is supplemented in youngster's food.
National standard GB10765-2010 " national food safety standard infant formula " regulation: l-carnitine is alternative adds
Enter ingredient, it is specified that minimum additive amount is 0.3mg/100KJ[5].Detection about l-carnitine in baby formula milk powder at present, state
It is designated as GB29989-2013[6], spectrophotometer method, but since developing solution configures complexity；Acetyl coenzyme A and acetylcarnitine transfer
Enzyme is unstable, often makes testing result poor repeatability, and detection limit is higher (0.6mg/100g).L-carnitine detection reported in the literature
Method mainly has enzyme development process[7-9], the chromatography of ions[10-11], high performance liquid chromatography[12-14]Deng.Relevant references information
It is as follows:
[1] McCarry JD, Brown NF. The mitochondrial carnitine palmitoyl
transferase system from concept to molecular analysis[J].Eu J Biochem,1997,
244:1-14.
[2] Vaz F M,Wanders R J. Carnitine biosynthesis in mammals[J].
Biochemistry Journal,361,361(1):417-429.
[3] Lahjouji K, Mitchell G A, Qureshi I A. Carnitinetransport by
organic cation transporters and systemic carnitinedeficiency[J]. Molecular
Genetics and Metabolism,2001,73(4)287-297.
[4] Goudriaan J R,Den Boer M A,Rensen P C,et al.CD 36 deficiencyin
mice impairs lipoprotein lipase-mediated triglyceride clearance [J].Journal
of Lipid Research,2005,46(6) 2175-2181.
[5] GB10765-2010 national food safety standard infant formula [S]
[6] in GB29989-2013 national food safety standard infant food and dairy products L-carnitine measurement [S]
[7] Jean Demarquoy, Beatrice Georges, CarolineRigault, et al.
Radioisotopic determination of L-carnitine content infoods commonly eaten in
Western countries [J] .Food Chemistry.2004,86 (1): 137-142.
[8] Knuttel-GustavsenSeline. The determination of L-carnitine in
Several food samples [J] .Food Chemistry, 2007,105 (2): 793-804.
[9] Wang Tianxi, Xiong Wenming, Lin Mengyong spectrophotometry measure the L-carnitine content Fujian [J] analysis in milk powder
Test, 2012,21 (1): 52-56.
[10] AikateriniKakou, Nikolaos C.Megoulas, Michael A. Koupparis.
Determination of L-carnitine in food supplement formulations using ion-pair
Chromatography with indirect conductimetric detection [ J ] .Journal of
Chromatography A, 2005,1 069 (2): 209-215.
[11] Zou Xiaoli, Zhou Yanyang, Qiao Rong, Li Yuanqian, Li Yan high-efficiency anion chromatography are quickly analyzed in health food
L-carnitine [ J ] health research .2011,40 (3): 358-364.
[12] Zhu Weixia, Yang Jizhou, Liu Yafeng, etc..The rp-hplc determination of L-carnitine in health care product
[J].Analysis test journal, 2008 (10): 1124-1127.
[13] Zhao Rong, Sun Kaiqi, Luo Rencai.IP RPHPLC measures carnitine in health food
[J] Chinese food health magazine, 2002,14 (4): 25-26.
[14] Gan Binbin, Li Shaohao .HPLC method measure L-carnitine in health food and contain quantifier elimination [J] China Health
Examine magazine, 2010 (7): 1688-1689.
Summary of the invention
It is surveyed the technical problem to be solved in the present invention is to provide a kind of using ultra performance liquid chromatography tandem mass spectrum fast quantification
Determine the method for l-carnitine in baby formula milk powder, not only operating procedure is simple, avoids object caused by complex steps
Loss, while having analysis speed fast, high sensitivity, reproducible outstanding feature.
In order to solve the above technical problems, the technical solution used in the present invention is as follows.
Utilize the method for l-carnitine in ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder, packet
Containing following key step:
A, LC-MS analysis pre-treatment operates: taking sample to be tested to be initially dissolved in concentrated hydrochloric acid, is then surpassed
Sound extracts, and it is spare to filter to take filtrate after alkali neutralization, prepares titer using l-carnitine standard items at the same time；
B, machine measures on LC-MS analysis: upper machine carries out liquid respectively for the resulting sample solution of step A and titer
The measurement of phase Spectrometry, analyses and compares and obtains the quantitative levels of l-carnitine in baby formula milk powder.
As a preferred technical solution of the present invention, this method includes following key step:
A, LC-MS analysis pre-treatment operates: carrying out series of processes to sample to be tested and prepares solution to be measured, simultaneously
Titer is prepared using standard items:
A-1, sample pre-treatments: the uniformly mixed baby formula milk powder sample to be measured merging triangle of 1.00g is accurately weighed
In bottle, the solution containing 0.5-2mmol hydrochloric acid is added, then ultrasonic extraction 10-30min adjusts pH to 4-5 with sodium hydroxide,
It is filtered after constant volume, filtrate is spare；
The preparation of A-2, titer: weigh l-carnitine sterling dilute step by step obtain concentration be 10ng/mL, 50ng/mL,
The standard working solution of 100ng/mL, 200ng/mL, 500ng/mL, 1000ng/mL；
B, machine measures on LC-MS analysis: the resulting sample solution of step A and standard working solution are gone up machine respectively
LC-MS analysis measurement is carried out, standard curve is made and the determination data of sample solution is compared, obtains baby children
The quantitative levels of l-carnitine in youngster's formula milk；Wherein:
B-1, chromatographic condition setting are as follows: chromatographic column is CORTECS HILIC, specification 3.0mm × 100mm, 2.7 μm, column temperature
20-30 DEG C, sample volume 1.5-2.5 μ L, flow velocity 0.2-0.4ml/min use methanol -0.1%(v/v) formic acid is mobile phase；
B-2, Mass Spectrometry Conditions setting are as follows: ion source is electron spray ESI ion source, and cation scan pattern, scanning mode is
Multiple-reaction monitoring MRM, capillary voltage 3-5KV, atomization gas and collision gas are High Purity Nitrogen, and dry gas stream speed is 5-20L/min,
Dry temperature degree is 200 DEG C or more.
As a preferred technical solution of the present invention, this method includes following key step:
A, LC-MS analysis pre-treatment operates: carrying out series of processes to sample to be tested and prepares solution to be measured, simultaneously
Titer is prepared using standard items:
A-1, sample pre-treatments: accurately weigh 1.00g(and be accurate to 0.1mg) uniformly mixed baby formula milk powder to be measured
10mL 0.1mol/L hydrochloric acid and 30mL water, ultrasonic extraction 15min, then with 4% hydrogen-oxygen is added in 100mL triangular flask in sample
Change sodium and adjust pH to 4.5, be settled to 100mL, filters, filtrate crosses 0.22 μm of filter membrane, spare；
The preparation of A-2, standard reserving solution: weighing l-carnitine 1.00000g in 100mL volumetric flask, and ultrapure water dissolution is fixed
Hold, mix, obtains the standard reserving solution that concentration is 10mg/mL；
The preparation of A-3, standard working solution: taking milk powder blank sample, carries out pre-treatment according to the method for step A-1, with
The filtrate arrived configures series standard working solution as solvent, and l-carnitine standard reserving solution is diluted step by step and obtains concentration as 10ng/
The standard working solution of mL, 50ng/mL, 100ng/mL, 200ng/mL, 500ng/mL, 1000ng/mL, matching while using；
B, machine measures on LC-MS analysis: the resulting sample solution of step A and standard working solution are gone up machine respectively
LC-MS analysis measurement is carried out, standard curve is made and the determination data of sample solution is compared, obtains baby children
The quantitative levels of l-carnitine in youngster's formula milk；Wherein:
B-1, chromatographic condition setting are as follows: chromatographic column is CORTECS HILIC, specification 3.0mm × 100mm, 2.7 μm, column temperature
25 DEG C, sample volume 2 μ L, flow velocity 0.3ml/min, using methanol -0.1%(v/v) formic acid, volume ratio 20:80 is mobile phase；
B-2, Mass Spectrometry Conditions setting are as follows: ion source is electron spray ESI ion source, and cation scan pattern, scanning mode is
Multiple-reaction monitoring MRM, capillary voltage 4KV, atomization gas and collision gas are High Purity Nitrogen, and dry gas stream speed is 10L/min, dry
Temperature degree is 350 DEG C.
As a preferred technical solution of the present invention, the design parameter of ultrasonic extraction operation in A-1 is walked are as follows: working frequency
40KHz, power 250W.
As a preferred technical solution of the present invention, in step B-2, the parameter of mass spectral analysis is as shown in the table:
It * is quota ion.
As a preferred technical solution of the present invention, sample to be tested uses baby formula milk powder quality-control sample, left-handed
Carnitine standard items use the product of purity > 98%, and concentrated hydrochloric acid is that analysis is pure, and sodium hydroxide is that analysis is pure, and glacial acetic acid is excellent pure grade,
Formic acid is chromatographically pure, and acetonitrile and methanol are chromatographically pure, and ultrapure water is experiment ultrapure water.
As a preferred technical solution of the present invention, sensing equipment uses the Agilent equipped with electric spray ion source
1290 LC/6420 MS liquid chromatograph-mass spectrometers, using KQ3200 DB type numerical control ultrasonic cleaner, acid base detemination
Using PB-10 pH meter, weighs operation and use AL 204-IC electronic balance and XS 2050U electronic analytical balance.
The beneficial effects of adopting the technical scheme are that the method for inspection of the invention not only operating procedure letter
It is single, the loss of object caused by complex steps is avoided, while having analysis speed fast, high sensitivity, reproducible is prominent
Feature out.Sample to be tested completes analysis, l-carnitine linear relationship within the scope of 10~1000.0ng/mL in 5min in the present invention
Well (r=0.9993), basic, normal, high three horizontal recovery of standard addition of method are 82.43%~96.91%, and relative standard is inclined
For difference 1.46%~5.65%, detection limit (S/N=3) and quantitative limit (S/N=10) are respectively 0.1 μ g/kg, 1.0 μ g/kg.The present invention
Technical solution be applicable not only to laboratory testing, enterprise's high-volume Quality Control detection, the characteristics of due to it quick and precisely, pole has can
The professional standard or even national standard for matching milk powder coherent detection for baby can be developed, have great importance and be worth.The present invention has
The embodiment that the specific test data of beneficial effect see below.
Detailed description of the invention
Fig. 1 shows l-carnitine content obtained by the different ultrasonic extraction times in embodiment 1.
Fig. 2 be in embodiment 4 HILIC column to more reaction detection chromatograms of l-carnitine.
Fig. 3 is the ESI/MS/MS mass spectrogram of l-carnitine in embodiment 5.
Specific embodiment
The present invention is described in detail in following embodiment.Various raw materials used in the present invention and items of equipment are conventional city
Product is sold, can be bought and be directly obtained by market.
Material, reagent and the instrument and equipment that the present invention uses are described below.Material: baby matches milk powder, quality-control sample.Reagent:
L-carnitine standard items: CAS 541-15-1, purity > 98%(sigma company)；Concentrated hydrochloric acid is to analyze the pure (Tianjin Li Anlongbohua
Medical chemistry Co., Ltd)；Sodium hydroxide is to analyze pure (Tianjin De En chemical reagent Co., Ltd)；Glacial acetic acid is excellent pure grade
(development in science and technology Co., Ltd is recovered in Tianjin)；Formic acid is chromatographically pure (Dikma company)；Acetonitrile and methanol are chromatographically pure
(Fisher chemical company)；Experiment (is obtained) with ultrapure water by Millipore Milli-Q system purification distilled water.Instrument
Device equipment: 1290 LC/6420 MS liquid chromatograph-mass spectrometer of Agilent (is furnished with electric spray ion source, U.S.'s peace is prompt
Human relations company)；KQ3200 DB type numerical control ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.)；(Beijing match of PB-10 pH meter
More Li Si instrument systems Co., Ltd)；AL 204-IC electronic balance, XS 2050U electronic analytical balance (Teller-support benefit instrument
Device Shanghai Co., Ltd).
The optimization of ultrasonic time is probed into embodiment 1, sample pre-treatments operation
Detection for l-carnitine in milk powder should guarantee the homogeneity of sample, reduce constant mesh in sample substrate again
Mark pollution of the compound to instrument.Part representative sample is taken out in research of the invention from original solid sample, is sufficiently mixed,
With quartering division, then sample is accurately weighed, hydrochloric acid solution is added and carries out ultrasonic extraction.Wherein the optimization of ultrasonic time is probed into
It is as follows.
Weighed respectively with a five parts of sample, after hydrochloric acid solution is added, respectively ultrasound 5min, 10min, 15min, 20min,
Then 25min is detected, final result of extracting is referring to attached drawing 1, it is seen that ultrasonic extraction time difference extraction effect is different, but 15min
Left and right reaches polyoptimal, therefore of the present invention group of final choice ultrasonic extraction 15min.
Final pH optimization is probed into embodiment 2, sample pre-treatments operation
PH gradient is adjusted with sodium hydroxide solution, 3.5,3.8,4.0,4.5,5.0,7.0, and upper machine testing l-carnitine respectively
Content, only when pH is 4.5, albumen precipitation is complete, filtrate clarification, and chromatographic peak profile is best in LC/MS/MS, therefore sample
It is determined as 4.5 to by final pH in product pre-treatment operation.
The optimization of sample extension rate is probed into embodiment 3, sample pre-treatments operation
Since LC/MS/MS instrumental sensitivity is high, it is necessary to which the dilution for making sample carry out certain multiple can just make L- in treatment fluid
Carnitine content is within the scope of the optimum linear of instrument.And dilution can also be such that the inhibition of sample substrate reduces, and make the noise of instrument
Than reducing, sensitivity is improved.Through overtesting final choice after treatment fluid constant volume 100ml, 0.22 μm of filter must also be crossed at this time
Film can be only achieved preferable measurement effect；It is optimal that gained filtrate, which dilutes 5 times with ultrapure water again,.
The optimization of embodiment 4, chromatographic condition is probed into
L-carnitine is a kind of highly polar compound of small molecule, not special UV absorption, and previous research all passes through
Derivatization reduces the polarity of l-carnitine anyway, more suitable for the reservation in antiphasic condition while making it with chromophore, originally
Experiment is not required to derive, and compared the separating effect of C18 column, C4 column and HILIC column respectively, discovery C18 column, C4 base for post sheet are when dead
Between appearance, and trailing phenomenon is serious, and HILIC column retention time is moderate, and peak shape is fine, sees attached drawing 2, is suitble to quantitative analysis.
The optimization of embodiment 5, Mass Spectrometry Conditions is probed into
Contain quaternary ammonium alkalinity group, suitable electric spray ion source, positive ion detection mode, L- in l-carnitine molecular structure
The quasi-molecular ion [M+H] of carnitine+Karyoplasmic ratio m/z is 162.2, is selected as parent ion and carries out next step collision-induced solution
From to collision energy, fragmentation voltage, dry gas stream speed, temperature optimizes.Second order ms show the most strong fragment of signal from
Sub- karyoplasmic ratio m/z is 103.1,85.2 and 60.3.By attached drawing 3 it is found that signal is up to that m/z103.1 fragment ion can be used as calmly
Ion is measured, followed by m/z60.3 is shown in Table 1 as qualitative ion, final mass spectral analysis parameter.In the detection process, using switching
Column effluent before l-carnitine appearance and after appearance is imported waste fluid channel, avoids leading to letter because of pollution of ion source by method
Number inhibit, signal-to-noise ratio reduce, improve the accuracy and sensitivity of instrument.
Embodiment 6, to the methodology validation of measuring method of the present invention
1, the range of linearity and detection limit
LC/MS/MS measurement is carried out with ultrapure water configuration l-carnitine concentration series standard solution, with each component response (Y)
Make standard curve with corresponding mass concentration (X).Experiment shows l-carnitine linear relationship within the scope of 10~1000ng/ml
Well, r=0.9993.It can satisfy the needs of quantitative analysis, as a result calculate and use quantified by external standard method.
Stock solution is taken to dilute step by step, 2 μ L of sample volume.With signal-to-noise ratio S/N=3 calculate l-carnitine detection limit (LOD) and S/N=
10 calculating quantitative limit (LOQ) are respectively 0.1 μ g/kg, 1 μ g/kg, can satisfy requirement of the actual sample analysis to detection limit.
2, the rate of recovery and precision
It takes baby with quality-control sample two of matrix powdered milk sample two and purchase respectively, measures L- meat therein by this method
Alkali background concentration.It is separately separately added into the standard items of 8.0,16.0,32.0mg/100g into powdered milk sample, distinguishes in quality-control sample
The standard items of 5.0,10.0,20.0mg/100g are added, each sample is measured in parallel 5 times, calculates its recovery of standard addition and opposite mark
Quasi- deviation, the results are shown in Table 2.As shown in Table 2, quality-control sample testing result meets error range with true value 9.9mg/100g.L- meat
The recovery of standard addition of alkali is 82.43%~96.91%, and relative standard deviation is 1.46%~5.65%.Method shows preferable return
Yield and repeatability can satisfy the analysis requirement of actual sample.
The rate of recovery and precision (n=5) of 2 l-carnitine of table
L-carnitine(n=5 Tab.2 Recovery and precision of)
3, method reproducibility
By same instrument, same laboratory technician, same quality-control sample is carried out continuously detecting 3d on the same day by this method, often
Its replication (n=5), investigates the reproducibility of method, and as a result the withinday precision of method is 2.6%, day to day precision 5.7%,
Show that method reproducibility is good.
In conclusion method of the invention is based on the efficient quick of sour water solution ultrasonic extraction, HPLC MS
High separation capacity and high sensitivity established a kind of suitable by the optimization to sample pre-treatments and liquid chromatography-mass spectrography condition
The Fast Detection Technique of l-carnitine for baby milk powder complex matrices.This method using CORTECS HILIC chromatographic column into
Row separation, using -0.1% formic acid of methanol as mobile phase, flow velocity 0.3ml/min, with optimal conditions, sample complete to divide in 5min
Analysis, analysis speed is fast, and l-carnitine linear relationship within the scope of 10~1000.0ng/mL is good, and detection limit is low.This method operation letter
Just, high sensitivity, reproducible, the quick measurement for the l-carnitine that can be used in a large amount of baby formula milk powder samples.
Foregoing description is only proposed as the enforceable technical solution of the present invention, not as to the single of its technical solution itself
Restrictive condition.
Claims (6)
1. special using the method for l-carnitine in ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder
Sign is: this method includes following key step:
A, LC-MS analysis pre-treatment operates: carrying out series of processes to sample to be tested and prepares solution to be measured, utilizes simultaneously
Standard items prepare titer:
A-1, sample pre-treatments: accurately weighing in the uniformly mixed baby formula milk powder sample to be measured merging triangular flask of 1.00g,
The solution containing 0.5-2mmol hydrochloric acid is added, then ultrasonic extraction 10-30min adjusts pH to 4-5 with sodium hydroxide, after constant volume
Filtering, filtrate are spare；
The preparation of A-2, titer: weigh l-carnitine sterling dilute step by step obtain concentration be 10ng/mL, 50ng/mL, 100ng/
The standard working solution of mL, 200ng/mL, 500ng/mL, 1000ng/mL；
B, machine measures on LC-MS analysis: by the resulting sample solution of step A and standard working solution, upper machine is carried out respectively
LC-MS analysis measurement makes standard curve and the determination data of sample solution is compared, show that infant matches
The quantitative levels of l-carnitine in square milk powder；Wherein:
B-1, chromatographic condition setting are as follows: chromatographic column is CORTECS HILIC, specification 3.0mm × 100mm, 2.7 μm, column temperature 20-30
DEG C, sample volume 1.5-2.5 μ L, flow velocity 0.2-0.4ml/min use -0.1% formic acid of methanol for mobile phase；
B-2, Mass Spectrometry Conditions setting are as follows: ion source is electron spray ESI ion source, and cation scan pattern, scanning mode is mostly anti-
MRM should be monitored, capillary voltage 3-5KV, atomization gas and collision gas are High Purity Nitrogen, and dry gas stream speed is 5-20L/min, dry
Temperature degree is 200 DEG C or more.
2. according to claim 1 utilize ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder
The method of middle l-carnitine, it is characterised in that: this method includes following key step:
A, LC-MS analysis pre-treatment operates: carrying out series of processes to sample to be tested and prepares solution to be measured, utilizes simultaneously
Standard items prepare titer:
A-1, sample pre-treatments: the uniformly mixed baby formula milk powder sample to be measured of 1.00g is accurately weighed in 100mL triangular flask
In, 10mL 0.1mol/L hydrochloric acid and 30mL water is added, then ultrasonic extraction 15min adjusts pH to 4.5 with 4% sodium hydroxide, fixed
Hold to 100mL, filtering, filtrate crosses 0.22 μm of filter membrane, spare；
The preparation of A-2, standard reserving solution: weighing l-carnitine 1.00000g in 100mL volumetric flask, and ultrapure water dissolves constant volume, mixes
It is even, obtain the standard reserving solution that concentration is 10mg/mL；
The preparation of A-3, standard working solution: taking milk powder blank sample, pre-treatment is carried out according to the method for step A-1, with what is obtained
Filtrate as solvent configure series standard working solution, l-carnitine standard reserving solution dilute step by step obtain concentration for 10ng/mL,
The standard working solution of 50ng/mL, 100ng/mL, 200ng/mL, 500ng/mL, 1000ng/mL；
B, machine measures on LC-MS analysis: by the resulting sample solution of step A and standard working solution, upper machine is carried out respectively
LC-MS analysis measurement makes standard curve and the determination data of sample solution is compared, show that infant matches
The quantitative levels of l-carnitine in square milk powder；Wherein:
B-1, chromatographic condition setting are as follows: chromatographic column is CORTECS HILIC, specification 3.0mm × 100mm, 2.7 μm, 25 DEG C of column temperature,
Sample volume 2 μ L, flow velocity 0.3ml/min, using -0.1% formic acid of methanol, volume ratio 20:80 as mobile phase；
B-2, Mass Spectrometry Conditions setting are as follows: ion source is electron spray ESI ion source, and cation scan pattern, scanning mode is mostly anti-
MRM should be monitored, capillary voltage 4KV, atomization gas and collision gas are High Purity Nitrogen, and dry gas stream speed is 10L/min, dry temperature
Degree is 350 DEG C.
3. according to claim 2 utilize ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder
The method of middle l-carnitine, it is characterised in that: the design parameter of ultrasonic extraction operation in step A-1 are as follows: working frequency 40KHz, power
250W。
4. according to claim 2 utilize ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder
The method of middle l-carnitine, it is characterised in that: in step B-2, the parameter of mass spectral analysis is as shown in the table:
It * is quota ion.
5. according to claim 2 utilize ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder
The method of middle l-carnitine, it is characterised in that: sample to be tested uses baby formula milk powder quality-control sample, and L-carnitine standard items are adopted
With the product of purity > 98%, concentrated hydrochloric acid is that analysis is pure, and sodium hydroxide is that analysis is pure, and glacial acetic acid is excellent pure grade, and formic acid is chromatographically pure,
Acetonitrile and methanol are chromatographically pure, and ultrapure water is experiment ultrapure water.
6. according to claim 2 utilize ultra performance liquid chromatography tandem mass spectrum quantitative determination baby formula milk powder
The method of middle l-carnitine, it is characterised in that: sensing equipment uses 1290 LC/6420 of Agilent equipped with electric spray ion source
MS liquid chromatograph-mass spectrometer, using KQ3200 DB type numerical control ultrasonic cleaner, acid base detemination uses PB-10 pH
Meter weighs operation and uses AL 204-IC electronic balance and XS 2050U electronic analytical balance.
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| CN107703204B (en) * | 2017-09-26 | 2021-09-14 | 中国检验检疫科学研究院 | Rapid detection method for forbidden pesticides in pesticide product |
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| CN113219097B (en) * | 2021-01-15 | 2022-06-24 | 杭州海关技术中心 | Method for splitting and measuring carnitine enantiomer in infant formula milk powder |
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| CN101975837A (en) * | 2010-09-07 | 2011-02-16 | 浙江大学 | Method for determining content and purity of L-carnitine in milk powder |
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