CN105352783A - Determination method of content of inorganic phosphorus in sodium phytate - Google Patents

Determination method of content of inorganic phosphorus in sodium phytate Download PDF

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Publication number
CN105352783A
CN105352783A CN201510922080.0A CN201510922080A CN105352783A CN 105352783 A CN105352783 A CN 105352783A CN 201510922080 A CN201510922080 A CN 201510922080A CN 105352783 A CN105352783 A CN 105352783A
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China
Prior art keywords
sodium phytate
content
inorganic phosphorus
percent
determination method
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CN201510922080.0A
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Chinese (zh)
Inventor
郭平
吕小丽
左海根
江龙发
于清丽
易明
祝建新
占春瑞
石磊
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Comprehensive Technology Center Jiangxi Entry And Exit Inspection And Quarantin
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Comprehensive Technology Center Jiangxi Entry And Exit Inspection And Quarantin
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Priority to CN201510922080.0A priority Critical patent/CN105352783A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

The invention discloses a determination method of the content of inorganic phosphorus in sodium phytate. The determination method comprises the following steps: firstly, adding a ferric trichloride solution into a sodium phytate sample solution to form sediment [C6H6(OH)H3(PO4)6]3Fe; removing base material influences of the sodium phytate by using a chelating effect of phytic acid and metal ions; centrifuging at a high speed to remove the sediment and adding a vanadate molybdate solution to generate a yellow phosphorus-vanadium molybdate coordination compound; determining a light absorption value at 420nm by using a spectrophotometer; calculating the content of the inorganic phosphorus in the sample according to a standard curve. According to the determination method provided by the invention, a base material effect is removed by using ferric trichloride and then a vanadium-molybdenum-yellow method is used for determining the content of the inorganic phosphorus; the method is reasonable and is simple and convenient to operate; the problems that the inorganic phosphorus in the sodium phytate is detected and has no recycling, and the base material interference is eliminated are solved; when the adding concentration is 0.02 percent to 0.08 percent, the recycling rate ranges from 99.0 percent to 102.48 percent, and the relative standard deviation is smaller than 1.16 percent; the technological indexes meet the requirements of GB/T 27404-2008 Food Physicochemical Detection of Laboratory Quality Control Standards.

Description

The assay method of content of inorganic phosphorus in a kind of sodium phytate
Technical field
The present invention relates to Phos detection technique field, specifically the assay method of content of inorganic phosphorus in a kind of sodium phytate.
Background technology
It is the sample only having Phos/organophosphorus that domestic current detection method major part is suitable for matrix; Detection method principle is molybdenum blue method and phosphorus molybdenum yellow method, but for this special sample solution of sodium phytate, when molybdenum blue method conveniently and phosphorus molybdenum yellow method carry out content of inorganic phosphorus detection, sample adds not recovery.
Summary of the invention
The assay method of content of inorganic phosphorus in the sodium phytate that the object of the present invention is to provide a kind of method reasonable, easy and simple to handle, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
An assay method for content of inorganic phosphorus in sodium phytate, first adds liquor ferri trichloridi in sodium phytate sample solution, makes it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, high speed centrifugation adds vanadium molybdenum acid solution after discarding precipitation again, generates yellow phosphovanadomolybdic acid complex, surveys its light absorption value, according to the content of Phos in typical curve calculation sample with spectrophotometer at 420nm place.
As the present invention's further scheme: described ultracentrifugal rotating speed is 7500-9500r/min.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts ferric trichloride to remove matrix effect and measures content of inorganic phosphorus with phosphorus molybdenum yellow method again, method is reasonable, easy and simple to handle, solving sodium phytate Phos detects without recovery, the problem getting rid of matrix interference, when interpolation concentration is 0.02-0.08%, recovery scope is between 99.0-102.48%, and relative standard deviation is all less than 1.16%, the requirement that methodology index meets " GB/T27404-2008 Good Laboratory controls specification food Physico-chemical tests ".
Embodiment
Be described in more detail below in conjunction with the technical scheme of embodiment to this patent.
Embodiment 1
An assay method for content of inorganic phosphorus in sodium phytate, first adds liquor ferri trichloridi in sodium phytate sample solution, makes it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, the matrix utilizing the chelation of phytic acid and metallic ion to remove sodium phytate affects, vanadium molybdenum acid solution is added again after high speed centrifugation discards precipitation under 7500r/min rotating speed, generate yellow phosphovanadomolybdic acid complex, its light absorption value is surveyed at 420nm place, according to the content of Phos in typical curve calculation sample with spectrophotometer.
Embodiment 2
An assay method for content of inorganic phosphorus in sodium phytate, first adds liquor ferri trichloridi in sodium phytate sample solution, makes it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, the matrix utilizing the chelation of phytic acid and metallic ion to remove sodium phytate affects, vanadium molybdenum acid solution is added again after high speed centrifugation discards precipitation under 8000r/min rotating speed, generate yellow phosphovanadomolybdic acid complex, its light absorption value is surveyed at 420nm place, according to the content of Phos in typical curve calculation sample with spectrophotometer.
Embodiment 3
An assay method for content of inorganic phosphorus in sodium phytate, first adds liquor ferri trichloridi in sodium phytate sample solution, makes it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, the matrix utilizing the chelation of phytic acid and metallic ion to remove sodium phytate affects, vanadium molybdenum acid solution is added again after high speed centrifugation discards precipitation under 8500r/min rotating speed, generate yellow phosphovanadomolybdic acid complex, its light absorption value is surveyed at 420nm place, according to the content of Phos in typical curve calculation sample with spectrophotometer.
Embodiment 4
An assay method for content of inorganic phosphorus in sodium phytate, first adds liquor ferri trichloridi in sodium phytate sample solution, makes it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, the matrix utilizing the chelation of phytic acid and metallic ion to remove sodium phytate affects, vanadium molybdenum acid solution is added again after high speed centrifugation discards precipitation under 9000r/min rotating speed, generate yellow phosphovanadomolybdic acid complex, its light absorption value is surveyed at 420nm place, according to the content of Phos in typical curve calculation sample with spectrophotometer.
Embodiment 5
An assay method for content of inorganic phosphorus in sodium phytate, first adds liquor ferri trichloridi in sodium phytate sample solution, makes it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, the matrix utilizing the chelation of phytic acid and metallic ion to remove sodium phytate affects, vanadium molybdenum acid solution is added again after high speed centrifugation discards precipitation under 9500r/min rotating speed, generate yellow phosphovanadomolybdic acid complex, its light absorption value is surveyed at 420nm place, according to the content of Phos in typical curve calculation sample with spectrophotometer.
The present invention adopts ferric trichloride to remove matrix effect and measures content of inorganic phosphorus with phosphorus molybdenum yellow method again, method is reasonable, easy and simple to handle, solving sodium phytate Phos detects without recovery, the problem getting rid of matrix interference, when interpolation concentration is 0.02-0.08%, recovery scope is between 99.0-102.48%, and relative standard deviation is all less than 1.16%, the requirement that methodology index meets " GB/T27404-2008 Good Laboratory controls specification food Physico-chemical tests ".
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, various change can also be made under the prerequisite not departing from this patent aim.

Claims (2)

1. the assay method of content of inorganic phosphorus in sodium phytate, is characterized in that, first in sodium phytate sample solution, add liquor ferri trichloridi, make it form precipitation [C 6h 6(OH) H 3(PO 4) 6] 3fe, high speed centrifugation adds vanadium molybdenum acid solution after discarding precipitation again, generates yellow phosphovanadomolybdic acid complex, surveys its light absorption value, according to the content of Phos in typical curve calculation sample with spectrophotometer at 420nm place.
2. the assay method of content of inorganic phosphorus in sodium phytate according to claim 1, it is characterized in that, described ultracentrifugal rotating speed is 7500-9500r/min.
CN201510922080.0A 2015-12-14 2015-12-14 Determination method of content of inorganic phosphorus in sodium phytate Pending CN105352783A (en)

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CN201510922080.0A CN105352783A (en) 2015-12-14 2015-12-14 Determination method of content of inorganic phosphorus in sodium phytate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758813A (en) * 2016-04-22 2016-07-13 广西中烟工业有限责任公司 Method for determining phosphate in cigarette paper

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1047675A (en) * 1989-05-30 1990-12-12 邓家璜 With luxuriant and rich with fragrance spit of fland is the method that raw material is produced phytic acid
US5734031A (en) * 1995-09-25 1998-03-31 The United States Of America As Represented By The Secretary Of Agriculture Cation exchange resin
CN101602777A (en) * 2009-07-03 2009-12-16 安徽丰原生物化学股份有限公司 A kind of method of extracting phytic acid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1047675A (en) * 1989-05-30 1990-12-12 邓家璜 With luxuriant and rich with fragrance spit of fland is the method that raw material is produced phytic acid
US5734031A (en) * 1995-09-25 1998-03-31 The United States Of America As Represented By The Secretary Of Agriculture Cation exchange resin
CN101602777A (en) * 2009-07-03 2009-12-16 安徽丰原生物化学股份有限公司 A kind of method of extracting phytic acid

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
REX ELLIS ET.AL: "Quantitative determination of phytate in the presence of high inorganic phosphate", 《ANALYTICAL BIOCHEMISTRY》 *
中国人民共和国国家质量监督检验检验检疫总局 等: "《中华人民共和国国家标准》", 31 August 2008 *
叶在荣 等: "总磷无机磷差值法测定植酸", 《贵州农学院学报》 *
周明义 等: "肌醇水解渣中植酸磷、无机磷、有机磷的测定", 《化学世界》 *
梁慧锋 等: "植酸钙的提纯及其植酸磷含量的测定", 《安徽农业科学》 *
罗星亮: "磷钒钼酸分光光度法测定磷酸盐", 《华北电力技术》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758813A (en) * 2016-04-22 2016-07-13 广西中烟工业有限责任公司 Method for determining phosphate in cigarette paper

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Application publication date: 20160224