CN107632080A - A kind of method for determining pentachlorophenol residual quantity in birds, beasts and eggs and fowls egg products - Google Patents
A kind of method for determining pentachlorophenol residual quantity in birds, beasts and eggs and fowls egg products Download PDFInfo
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Abstract
A kind of method for determining pentachlorophenol residual quantity in birds, beasts and eggs and fowls egg products.It is characterized in that：1.0~5.0g of homogeneous sample is taken in 10mL polypropylene centrifuge tubes, add 5~15mL of acetonitrile solution containing 5.0%~10.0% (V/V) triethylamine, after ultrasonic extraction centrifuges, blended type anion exchange pillar (6mL) purification of supernatant, using the methanol/water solution (50/50 containing 1.0%~5.0%% (V/V) formic acid, V/V) eluted, eluted by several times with the methanol solution containing 6.0%~15.0% (V/V) formic acid, eluent is blown in 40 DEG C of nitrogen and closely done, and liquid chromatography tandem mass spectroscopy is supplied after being redissolved with methanol.Not only technique is simple and convenient to operate fast the present invention, and bioaccumulation efficiency is good, extraction recovery is high, cheap, with good detection sensitivity and precision, it is suitable for pentachlorophenol residue analysis in birds, beasts and eggs and fowls egg products, for pentachlorophenol residual quantity in control birds, beasts and eggs and fowls egg products, ensure food security and health of human body, have great importance.
Description
Technical field
The invention belongs to technical field of food safety detection, is related to a kind of for determining pentachlorophenol in birds, beasts and eggs and fowls egg products
The method of residual quantity, the extraction remained more specifically to pentachlorophenol in birds, beasts and eggs and fowls egg products, pillar enrichment purification and liquid
Phase chromatogram-tandem mass spectrometry measure.
Background technology
Pentachlorophenol (PCP) is mutagen, Insecticides (tech) ＆ Herbicides (tech), antiseptic and timber preservative is widely used as, in environment
The great attention of food security expert is caused with the presence in food.The birds, beasts and eggs protein food source main as the mankind it
One, due to being polluted in feeding process by environment and feed, often detection remains containing pentachlorophenol in birds, beasts and eggs.
At present, though the detection that pentachlorophenol remains in food has, " pentachlorophenol is residual in national food safety standard animal-derived food
The documents such as the measure liquid chromatography-mass spectrometry of allowance " (GB23200.92-2016), but many deficiencies still be present in existing literature：
First, absolute recovery is low, the sample extraction of for example international method of existing literature " uses the acetonitrile-water of 5% triethylamine
Solution is as extract solution ", although, being directed to birds, beasts and eggs and fowls egg products to lean meat, skim milk etc. more effectively, extraction it is absolute
The rate of recovery is very low, it is difficult to meets the detection limit requirement of method；
Second, matrix interference is big, existing literature method majority is purified using MAX pillars, but is directed to birds, beasts and eggs and birds, beasts and eggs system
Product, the elution of existing literature method and elution program are unable to reach preferable clean-up effect, matrix interference when causing Mass Spectrometer Method
It is larger, influence the accuracy of testing result.
Therefore a kind of simple, practical, quick extracting method and detection method are developed, for control birds, beasts and eggs and fowls egg products
Middle pentachlorophenol residual quantity, ensure food security and health of human body, have great importance.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of technique and are simple and convenient to operate, Sync enrichment efficiency high
Method for determining pentachlorophenol residual quantity in birds, beasts and eggs and fowls egg products.
Technical scheme is used by the present invention solves above-mentioned technical problem：One kind is used to determine in birds, beasts and eggs and fowls egg products
The method of pentachlorophenol residual quantity, it is characterised in that comprise the following steps：
1) extract：Take representative birds, beasts and eggs and fowls egg products sample, fully mix after weigh 1.0~5.0g in one from
In heart pipe, 4~6 μ L 1.0mg/L is added13C6- PCP internal standards contain 5.0%~10.0% (V/V) three using liquid and 5~15mL's
The acetonitrile-aqueous solution (60~80/40~20, V/V) of ethamine, homogenate, 5~15min of ultrasonic extraction, be vortexed 5~15min, topples over
Go out supernatant in another centrifuge tube, then 8000~9000r/min centrifuges 4~6min, draws 4~6mL supernatants and is filled in tool
In test tube, 1.5~2.5mL water is added, it is to be clean after mixing；
2) enrichment purification：Said extracted liquid is added with water and methanol activation and the mixed type anion exchange of balance
In pillar, 1.5~2.5mL/min of coutroi velocity, then respectively with methanol, water and containing 1.0%~5.0% (V/V) formic acid
Methanol/water solution (50/50, V/V) is eluted, and the methanol solution containing 6.0%~15.0% (V/V) formic acid is used after drying by several times
Elution, and collect, eluent is blown in 35~45 DEG C of nitrogen and closely done, and is redissolved with methanol and is settled to 1.0mL, through 0.18~0.22
After μm membrane filtration, for liquid chromatography tandem mass spectroscopy.
Preferably, the birds, beasts and eggs and fowls egg products are one kind in egg, duck's egg, quail egg or cake.
Preferably, the volume ratio of the acetonitrile-aqueous solution in the step 1) is 60:40、70:30、80:One in 20
Kind, the volume ratio of triethylamine and acetonitrile-aqueous solution is 5~10 in the mixed liquor of triethylamine-(acetonitrile-aqueous solution):100.
Further preferably, the volume ratio of the acetonitrile-aqueous solution is 70:30, the volume ratio of triethylamine and acetonitrile-aqueous solution
For 8:100.
As an improvement, the filler that mixed type anion exchange pillar in the step 2) uses be magnetic it is aminated it is cloudy from
Son exchanges composite and common C18 fillers mix by weight 70mg/30mg, 80mg/20mg, 90mg/10mg, 100mg/0mg
Conjunction forms, and pillar is to load to form using 6mL blank pipes, amount of filler 150mg, for the methanol of elution, water and containing 1.0%~
The methanol/water solution of 5.0% (V/V) formic acid is 6mL.
Improve again, the aminated anion exchange composite of magnetic is that one kind uses NVP and four
The composite wood that the amine of ethene five (TEPA) obtains in the aggregated reaction in the magnetic ferroferric oxide surface of coated silica
Material, the composite is spherical, a diameter of 30~80 μm, 300~600m of specific surface area2/ g, carbon carrying capacity 2~5%, exchange capacity
0.5~2meq/g, the weight ratio of the aminated anion exchange composite of magnetic and common C18 fillers is 80mg/20mg.
Preferably, in the step 2) containing 1.0%~5.0% (V/V) formic acid methanol/water solution in formic acid content
For one kind in 1.0%, 2.0%, 3.0%, 4.0% and 5.0% (V/V)；Methanol containing 6.0%~15.0% (V/V) formic acid
The content of formic acid is 6.0%, 7.0%, 8.0%, 9.0%, 10.0%, 11.0%, 12.0%, 13.0%, 14.0% in solution
With one kind in 15.0% (V/V).
Further preferably, the methanol/water solution (50/50, V/ of 1.0%~5.0% (V/V) formic acid is contained in the step 2)
V the content of formic acid is 2.0% in)；The content of formic acid is 10.0% in methanol solution containing 6.0%~15.0% (V/V) formic acid.
Further improve, the Liquid Chromatography-Tandem Mass Spectrometry analysis analysis uses XR-ODS III (150mm × 2.1mm
I.d., 2.2 μm) post, with the aqueous solution of ammonium acetate containing 5mmol/L and 0.1% formic acid (A phases) and ammonium acetate containing 5mmol/L and
The acetonitrile solution (B phases) of 0.1% formic acid is that mobile phase carries out gradient elution.
Finally, the program of the gradient elution：0~1.00min：40%~90% (B phases), 1.00~3.00min：90%
(B phases), 3.00~3.01min：90%~40% (B phases), 3.01~5.00min：40% (B phases)；Ion gun：Electron spray ionisation
(ESI)；Scan mode：Anion scans；Quantitative manner：Multiple-reaction monitoring pattern (MRM), Internal standard；PCP it is quantitative from
Son is to (m/z)：264.8>35.0 266.8>35.0；13C6- PCP quota ion pairs (m/z)：270.8>35.0 272.8>35.0；
Ion source temperature (TEM)：500℃；Sweep time：50ms；Collision cell exit potential (CXP)：10.0V；Collision cell entrance potential
(EP)：10.0V.
Compared with prior art, the advantage of the invention is that：
First, extracted using the acetonitrile-water mixed solution of 5.0%~10.0% (V/V) triethylamine in birds, beasts and eggs and fowls egg products
The trace pentachlorophenol of residual, overcomes the problem of pentachlorophenol extraction recovery is low in existing extracting method；
2nd, enrichment purification is carried out to extract solution using mixed type anion exchange pillar, overcomes and be enriched with the prior art
The problem of purification is not thorough, Mass Spectrometer Method matrix interference is serious；
3rd, using 6.0%~15.0% (V/V) formic acid methanol solution elute, overcome elute in the prior art it is endless
The problem of complete, elution efficiency is substantially increased, reduce detection limit, make the detection of trace pentachlorophenol in birds, beasts and eggs and fowls egg products more
Accurately, it is as a result more reliable；
Not only technique is simple and convenient to operate fast the present invention, and extraction recovery is high, cheap, is had well
Detection sensitivity and precision, it is suitable for pentachlorophenol residue analysis in birds, beasts and eggs and fowls egg products, for control birds, beasts and eggs and birds, beasts and eggs
Pentachlorophenol residual quantity in product, ensure food security and health of human body, have great importance.
Brief description of the drawings
Fig. 1 is pentachlorophenol (a, b) and 13C in 1-6 of the embodiment of the present invention6The MRM figures of-pentachlorophenol (c, d)；
Fig. 2 be 1-6 of the embodiment of the present invention in pentachlorophenol (a, b) and13C6- pentachlorophenol (c, d) second order mses figure；
Fig. 3 is that pentachlorophenol egg mark-on sample MRM schemes in the embodiment of the present invention 1.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1
First, representative egg sample is taken, is cooked, 2.0g is weighed after fully mixing in 50mL centrifuge tubes, adds 5
μ L's13C6- PCP internal standards use liquid (1.0mg/L), and the acetonitrile solution (70/30, V/V) for adding 8% (V/V) triethylamine carries
Liquid 10mL is taken, is homogenized 1min, ultrasonic extraction 10min, vortex 10min, then 8500r/min centrifuges 5min, draws 5mL supernatants
In in tool plug test tube, addition 2mL water is to be clean after mixing.
2nd, said extracted liquid is added with 5mL methanol and the activation of 5mL water and the mixed type anion exchange pillar of balance
(6mL/150mg), the aminated anion exchange composite of magnetic and common C18 fillers are by weight 80mg/20mg), control
Flow velocity 2mL/min, then entered respectively with formic acid/methanol/water solution (2/49/49, V/V/V) of 6mL methanol, 6mL water and 6mL
Row elution, uses the methanol solution 10mL containing 10% (V/V) formic acid to elute by several times after drying, collects eluent, is blown in 40 DEG C of nitrogen
Done near, redissolved with methanol and be settled to 1.0mL, after 0.2 μm of membrane filtration, for liquid chromatography tandem mass spectroscopy (pentachloro-
The MRM figures and second order mses figure of phenol are shown in Fig. 1 and Fig. 2 respectively).As a result measure recovery of standard addition in egg for 82.6~
98.1%.
The parameter of the present embodiment is changed to illustrate optimal processing parameter below：
Above-mentioned other conditions are constant, change said extracted liquid in triethylamine volume ratio, respectively 5.0%, 6.0%,
7.0%th, 8.0%, 9.0% and 10.0% (V/V), is then tested respectively, is as a result measured when the ratio of triethylamine is 8.0%
When, the rate of recovery highest of pentachlorophenol in egg.
Above-mentioned other conditions are constant, change the aminated anion exchange composite of magnetic and common C18 fillers in pillar
The weight ratio of addition, respectively by the aminated anion exchange composite of magnetic and common C18 fillers by weight 70mg/
30mg, 80mg/20mg, 90mg/10mg, 100mg/0mg, above-mentioned mixed fillers 150mg is loaded in 6mL blank pipes, is carried out respectively
Experiment, when as a result the aminated anion exchange composite of magnetic and common C18 fillers are by weight 80mg/20mg, in egg
The recovery of standard addition of pentachlorophenol is up to 98.1%.
Above-mentioned other conditions are constant, change the content of formic acid in eluant, eluent (methanol solution containing formic acid), are respectively
6.0%th, carried out when 7.0%, 8.0%, 9.0%, 10.0%, 11.0%, 12.0%, 13.0%, 14.0% and 15.0% (V/V)
Experiment, as a result when the content of formic acid in eluant, eluent is 10.0%, the recovery of standard addition highest of pentachlorophenol, matrix interference in egg
Minimum, the matrix mark-on sample chromatogram figure of egg are shown in Fig. 3.
Embodiment 2
First, representative duck's egg sample is taken, is cooked, 2.0g is weighed after fully mixing in 50mL centrifuge tubes, adds 5
μ L's13C6- PCP internal standards use liquid (1.0mg/L), and the acetonitrile solution (70/30, V/V) for adding 8% (V/V) triethylamine carries
Liquid 10mL is taken, is homogenized 1min, ultrasonic extraction 10min, vortex 10min, then 8500r/min centrifuges 5min, draws 5mL supernatants
In in tool plug test tube, addition 2mL water is to be clean after mixing.
2nd, said extracted liquid is added with 5mL methanol and the activation of 5mL water and the mixed type anion exchange pillar of balance
(6mL/150mg, the aminated anion exchange composite of magnetic and common C18 fillers are by weight 80mg/20mg), controlling stream
Fast 2mL/min, then carried out respectively with formic acid/methanol/water solution (2/49/49, V/V/V) of 6mL methanol, 6mL water and 6mL
Elution, use the methanol solution 10mL containing 10% (V/V) formic acid to elute by several times after drying, collect eluent, be blown in 40 DEG C of nitrogen
It is near dry, redissolved with methanol and be settled to 1.0mL, after 0.2 μm of membrane filtration, for liquid chromatography tandem mass spectroscopy (pentachlorophenol
MRM figure and second order mses figure see Fig. 1 and Fig. 2 respectively).As a result it is 84.3~95.8% to measure the recovery of standard addition in duck's egg.
Embodiment 3：
First, representative quail egg sample is taken, is cooked, 2.0g is weighed in 50mL centrifuge tubes after fully mixing, adds
Enter 5 μ L's13C6- PCP internal standards use liquid (1.0mg/L), add the acetonitrile solution (70/30, V/V) of 8% (V/V) triethylamine
Extract solution 10mL, 1min, ultrasonic extraction 10min, vortex 10min are homogenized, then 8500r/min centrifuges 5min, draws 5mL supernatants
For liquid in tool plug test tube, addition 2mL water is to be clean after mixing.
2nd, said extracted liquid is added with 5mL methanol and the activation of 5mL water and the mixed type anion exchange pillar of balance
(6mL/150mg, the aminated anion exchange composite of magnetic and common C18 fillers are by weight 80mg/20mg), controlling stream
Fast 2mL/min, then carried out respectively with formic acid/methanol/water solution (2/49/49, V/V/V) of 6mL methanol, 6mL water and 6mL
Elution, use the methanol solution 10mL containing 10% (V/V) formic acid to elute by several times after drying, collect eluent, be blown in 40 DEG C of nitrogen
It is near dry, redissolved with methanol and be settled to 1.0mL, after 0.2 μm of membrane filtration, for liquid chromatography tandem mass spectroscopy (pentachlorophenol
MRM figure and second order mses figure see Fig. 1 and Fig. 2 respectively).As a result measure recovery of standard addition in quail egg for 85.6~
94.7%.
Embodiment 4：
First, representative cake sample is taken, is cooked, 2.0g is weighed after fully mixing in 50mL centrifuge tubes, adds 5
μ L's13C6- PCP internal standards use liquid (1.0mg/L), and the acetonitrile solution (70/30, V/V) for adding 8% (V/V) triethylamine carries
Liquid 10mL is taken, is homogenized 1min, ultrasonic extraction 10min, vortex 10min, then 8500r/min centrifuges 5min, draws 5mL supernatants
In in tool plug test tube, addition 2mL water is to be clean after mixing.
2nd, said extracted liquid is added with 5mL methanol and the activation of 5mL water and the mixed type anion exchange pillar of balance
(6mL/150mg, the aminated anion exchange composite of magnetic and common C18 fillers are by weight 80mg/20mg), controlling stream
Fast 2mL/min, then carried out respectively with formic acid/methanol/water solution (2/49/49, V/V/V) of 6mL methanol, 6mL water and 6mL
Elution, use the methanol solution 10mL containing 10% (V/V) formic acid to elute by several times after drying, collect eluent, be blown in 40 DEG C of nitrogen
It is near dry, redissolved with methanol and be settled to 1.0mL, after 0.2 μm of membrane filtration, for liquid chromatography tandem mass spectroscopy (pentachlorophenol
MRM figure and second order mses figure see Fig. 1 and Fig. 2 respectively).As a result it is 87.3~98.4% to measure the recovery of standard addition in cake.
Embodiment 5：
First, representative egg sample is taken, is cooked, 2.0g is weighed after fully mixing in 50mL centrifuge tubes, adds 5
μ L's13C6- PCP internal standards use liquid (1.0mg/L), and the acetonitrile solution (70/30, V/V) for adding 5% (V/V) triethylamine carries
Liquid 10mL is taken, is homogenized 1min, ultrasonic extraction 10min, vortex 10min, then 8500r/min centrifuges 5min, draws 5mL supernatants
In in tool plug test tube, addition 2mL water is to be clean after mixing.
2nd, said extracted liquid is added with 5mL methanol and the activation of 5mL water and the mixed type anion exchange pillar of balance
(6mL/150mg, the aminated anion exchange composite of magnetic and common C18 fillers are by weight 80mg/20mg), controlling stream
Fast 2mL/min, then carried out respectively with formic acid/methanol/water solution (2/49/49, V/V/V) of 6mL methanol, 6mL water and 6mL
Elution, use the methanol solution 10mL containing 8% (V/V) formic acid to elute by several times after drying, collect eluent, be blown to closely in 40 DEG C of nitrogen
It is dry, redissolved with methanol and be settled to 1.0mL, after 0.2 μm of membrane filtration, for liquid chromatography tandem mass spectroscopy (pentachlorophenol
MRM schemes and second order mses figure is shown in Fig. 1 and Fig. 2 respectively).As a result it is 43.6~52.5% to measure the recovery of standard addition in egg.
Embodiment 6：
First, representative duck's egg sample is taken, is cooked, 2.0g is weighed after fully mixing in 50mL centrifuge tubes, adds 5
μ L's13C6- PCP internal standards use liquid (1.0mg/L), and the acetonitrile solution (70/30, V/V) for adding 6% (V/V) triethylamine carries
Liquid 10mL is taken, is homogenized 1min, ultrasonic extraction 10min, vortex 10min, then 8500r/min centrifuges 5min, draws 5mL supernatants
In in tool plug test tube, addition 2mL water is to be clean after mixing.
2nd, said extracted liquid is added with 5mL methanol and the activation of 5mL water and the mixed type anion exchange pillar of balance
(6mL/150mg, the aminated anion exchange composite of magnetic and common C18 fillers are by weight 70mg/30mg), controlling stream
Fast 2mL/min, then carried out respectively with formic acid/methanol/water solution (2/49/49, V/V/V) of 6mL methanol, 6mL water and 6mL
Elution, use the methanol solution 10mL containing 7% (V/V) formic acid to elute by several times after drying, collect eluent, be blown to closely in 40 DEG C of nitrogen
It is dry, redissolved with methanol and be settled to 1.0mL, after 0.2 μm of membrane filtration, for liquid chromatography tandem mass spectroscopy (pentachlorophenol
MRM schemes and second order mses figure is shown in Fig. 1 and Fig. 2 respectively).As a result it is 42.7~58.3% to measure the recovery of standard addition in duck's egg.
Claims (10)
- A kind of 1. method for determining pentachlorophenol residual quantity in birds, beasts and eggs and fowls egg products, it is characterised in that comprise the following steps：1) extract：Representative birds, beasts and eggs and fowls egg products sample are taken, 1.0~5.0g is weighed in a centrifuge tube after fully mixing In, 4~6 μ L of addition 1.0mg/L13C6- PCP internal standards contain 5.0%~10.0% (V/V) triethylamine using liquid and 5~15mL's Acetonitrile-aqueous solution (60~80/40~20, V/V), homogenate, 5~15min of ultrasonic extraction, be vortexed 5~15min, pour out Clear liquid is in another centrifuge tube, and then 8000~9000r/min centrifuges 4~6min, draws 4~6mL supernatants in tool plug test tube It is interior, 1.5~2.5mL water is added, it is to be clean after mixing；2) enrichment purification：Said extracted liquid is added with water and the mixed type anion exchange pillar of methanol activation and balance In, 1.5~2.5mL/min of coutroi velocity, then respectively with methanol, water and methanol containing 1.0%~5.0% (V/V) formic acid/ The aqueous solution (50/50, V/V) is eluted, and uses the methanol solution containing 6.0%~15.0% (V/V) formic acid to elute by several times after drying, And collect, eluent is blown in 35~45 DEG C of nitrogen and closely done, and is redissolved with methanol and is settled to 1.0mL, through 0.18~0.22 μm of filter After membrane filtration, for liquid chromatography tandem mass spectroscopy.
- 2. according to the method for claim 1, it is characterised in that：The birds, beasts and eggs and fowls egg products are egg, duck's egg, quail egg Or one kind in cake.
- 3. according to the method for claim 1, it is characterised in that：The volume ratio of acetonitrile-aqueous solution in the step 1) is 60:40、70:30、80:One kind in 20, triethylamine and acetonitrile-aqueous solution in the mixed liquor of triethylamine-(acetonitrile-aqueous solution) Volume ratio is 5~10:100.
- 4. according to the method for claim 3, it is characterised in that：The volume ratio of the acetonitrile-aqueous solution is 70:30, three second The volume ratio of amine and acetonitrile-aqueous solution is 8:100.
- 5. according to the method for claim 1, it is characterised in that：Mixed type anion exchange pillar in the step 2) is adopted Filler is the aminated anion exchange composite of magnetic and common C18 fillers by weight 70mg/30mg, 80mg/ 20mg, 90mg/10mg, 100mg/0mg are mixed, and pillar is to load to form using 6mL blank pipes, amount of filler 150mg, is used for The methanol of elution, water and methanol/water solution containing 1.0%~5.0% (V/V) formic acid are 6mL.
- 6. according to the method for claim 5, it is characterised in that：The aminated anion exchange composite of magnetic is one Kind uses NVP and TEPA (TEPA) in the magnetic ferroferric oxide table of coated silica The aggregated reaction in face and the composite obtained, the composite is spherical, a diameter of 30~80 μm, and specific surface area 300~ 600m2/ g, carbon carrying capacity 2~5%, 0.5~2meq/g of exchange capacity, the aminated anion exchange composite of magnetic with it is common The weight ratio of C18 fillers is 80mg/20mg.
- 7. according to the method for claim 1, it is characterised in that：Contain 1.0%~5.0% (V/V) formic acid in the step 2) Methanol/water solution in formic acid content be 1.0%, 2.0%, 3.0%, 4.0% and 5.0% (V/V) in one kind；Contain In the methanol solution of 6.0%~15.0% (V/V) formic acid the content of formic acid be 6.0%, 7.0%, 8.0%, 9.0%, 10.0%, 11.0%th, one kind in 12.0%, 13.0%, 14.0% and 15.0% (V/V).
- 8. according to the method for claim 7, it is characterised in that：Contain 1.0%~5.0% (V/V) formic acid in the step 2) Methanol/water solution (50/50, V/V) in formic acid content be 2.0%；Methanol containing 6.0%~15.0% (V/V) formic acid is molten The content of formic acid is 10.0% in liquid.
- 9. according to the method for claim 1, it is characterised in that：The Liquid Chromatography-Tandem Mass Spectrometry analysis analysis uses XR- ODS III (150mm × 2.1mmi.d., 2.2 μm) post, with the aqueous solution of ammonium acetate containing 5mmol/L and 0.1% formic acid (A phases) and The acetonitrile solution of ammonium acetate containing 5mmol/L and 0.1% formic acid (B phases) is that mobile phase carries out gradient elution.
- 10. according to the method for claim 9, it is characterised in that：The program of the gradient elution：0-1.00min：40%~ 90% (B phases), 1.00-3.00min：90% (B phases), 3.00-3.01min：90%~40% (B phases), 3.01-5.00min： 40% (B phases)；Ion gun：Electron spray ionisation (ESI)；Scan mode：Anion scans；Quantitative manner：Multiple-reaction monitoring pattern (MRM), Internal standard；PCP quota ion pairs (m/z)：264.8>35.0 266.8>35.0；13C6- PCP quota ion pairs (m/z)：270.8>35.0 272.8>35.0；Ion source temperature (TEM)：500℃；Sweep time：50ms；Collision cell outlet electricity Press (CXP)：10.0V；Collision cell entrance potential (EP)：10.0V.
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| CN111505152A (en) * | 2020-05-06 | 2020-08-07 | 重庆大学 | Method for measuring residual amount of pentachlorophenol in pig hair |
| CN112305127A (en) * | 2020-11-09 | 2021-02-02 | 武汉工控检验检测有限公司 | LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) determination method for sodium pentachlorophenate residue in eggs |
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| CN111505152B (en) * | 2020-05-06 | 2022-11-15 | 重庆大学 | Method for measuring residual amount of pentachlorophenol in pig hair |
| CN112305127A (en) * | 2020-11-09 | 2021-02-02 | 武汉工控检验检测有限公司 | LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) determination method for sodium pentachlorophenate residue in eggs |
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