CN103033574B - Method for detecting residual solvent in subcritical propane extraction product - Google Patents

Method for detecting residual solvent in subcritical propane extraction product Download PDF

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CN103033574B
CN103033574B CN201210545709.0A CN201210545709A CN103033574B CN 103033574 B CN103033574 B CN 103033574B CN 201210545709 A CN201210545709 A CN 201210545709A CN 103033574 B CN103033574 B CN 103033574B
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propane
oil
standard
gas
sample
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CN103033574A (en
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徐斌
姜松
周世龙
董英
孙俊
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HENAN YALINJIE BIOLOGICAL TECHNOLOGY Co Ltd
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Jiangsu University
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Abstract

本发明涉及亚临界丙烷萃取产品中溶剂残留的检测方法,涉及食品安全检测领域。是先将丙烷标准气通入与待测油相同油种但不含丙烷的成品油中,充分稳定,准确称量,得到该储备液的浓度,然后将其稀释配制一系列丙烷标准油溶液,取该系列标准油溶液5.00~100.00g置于135mL顶空瓶中,在40~70℃恒温水浴条件下以500rpm的转速搅拌平衡10~60min,用微量进样器取其上层气体进行顶空气相色谱分析,相同条件下测待测油样品中残留丙烷峰面积,根据标准曲线,即可求得油样品中残留丙烷含量。该方法成本低、操作简便以及专属性强等优点,可广泛应用于油脂的亚临界流体加工企业及粮油检测机构的粮油品质检验与控制。

The invention relates to a detection method for solvent residues in subcritical propane extraction products, and relates to the field of food safety detection. The method is to inject the propane standard gas into the refined oil of the same type as the oil to be tested but without propane, fully stabilize and accurately weigh to obtain the concentration of the stock solution, and then dilute it to prepare a series of propane standard oil solutions. Take 5.00~100.00g of this series of standard oil solutions and place them in a 135mL headspace bottle, stir and balance at a speed of 500rpm in a constant temperature water bath at 40~70℃ for 10~60min, and use a micro sampler to take the upper layer gas for headspace phase For chromatographic analysis, the residual propane peak area in the oil sample to be tested is measured under the same conditions, and the residual propane content in the oil sample can be obtained according to the standard curve. The method has the advantages of low cost, simple operation and strong specificity, and can be widely used in the inspection and control of grain and oil quality in oil subcritical fluid processing enterprises and grain and oil testing institutions.

Description

The detection method of dissolvent residual in Propane extracted products
Technical field
The present invention relates to field of detection of food safety, refer in particular to a kind of method adopting gas chromatography to detect dissolvent residual in the edible oil and fat product of Propane fluid extraction fast, the method can be grease production enterprise and Safety of Food Quality testing agency supplying method foundation.
Background technology
Subcritical fluids refers to that some compound is higher than its boiling point but lower than under the condition of critical temperature and emergent pressure, the material existed with fluid form.Subcritical fluid extraction technology is then for solvent with subcritical fluids or its mixed solution, a kind of new technology of target components is extracted from natural products, be particularly suitable for the extraction of volatile oil in natural products, grease or liposoluble constituent, the change technology there is normal temperature leaching, low temperature desolventizing, do not destroy the outstanding advantage of heat-sensitive ingredients, be an environmental protection, having a extensive future.
The subcritical fluids being usually used in valuable grease production or effective components from natural materials extraction comprises: propane, butane, liquefied petroleum gas (LPG) (LPG), high-purity isobutane (R600a), 1,1,1,2-HFC-134a (R134a), dimethyl ether (DME) and sulfur hexafluoride etc., be wherein most widely used with propane, butane, LPG.The Ministry of Public Health of China includes propane in food processing aid catalogue in 2008, but has hypotoxicity due to it to nerve system of human body, so, be a food-safety problem that can not be ignored with dissolvent residual in the product of Propane extraction.
At present, Propane extraction grease in propane residue detection there is no unified national standard.Due to not enough to its attention degree, so far the research of the detection method about propane in grease is not had, and mensuration being most widely used with headspace gas chromatography of dissolvent residual in the vegetable oil products of conventional solvent extraction, GB5009.37-2003 just adopts this method to detect the residual quantity of No. six solvents.But because be gaseous state under propane normal temperature and pressure, and normal hexane is in a liquid state, and in contrast, it can not dissolve each other preferably with grease, makes the standard oil solution accurately cannot preparing propane, thus hinders the quantitative detection of residual propane in grease.
The people such as Xu Yun report the method with the propane in infrared spectrophotometer and Headspace-Gas Chromatography Analysis wastewater measurement, butane.Although this method determines the content of propane in waste water, butane.But researchist is not mixed with standard items by soluble in water for propane, but directly with the Standard Gases sample introduction of variable concentrations, the matrix of standard items and testing sample is inconsistent, causes the inaccurate of measurement, matrix simultaneously containing propane compared with grease is different, because the method is inadvisable.
For this reason, two key technical problems must be solved: first when adopting headspace gas chromatography to detect dissolvent residual in Propane extracted products, when preparation standard solution, propane can dissolve each other well with matrix oil, accurately could obtain variable concentrations (series) propane solution; Secondly, the matrix of standard solution must be consistent with the matrix of testing sample, and like this, the concentration that both balance rear headspace gas just has comparability.
In order to solve above-mentioned two key technical problems, propane calibrating gas first passes in the matrix oil (not containing propane) same with oil phase to be measured by the present invention, make it be fully absorbed, then above-mentioned propane solution is carried out uncovered be placed to stable, diluted again, thus preparation obtains a series of propane standard oil solution.
Summary of the invention
The present invention solves the technical scheme that its detection technique adopts: take not containing the product oil of propane, propane is passed in this product oil, stop after a period of time passing into propane gas, weigh the quality of product oil after a period of stabilisation, obtain the concentration of propane in this oil; Then a certain amount of above-mentioned propane solution product oil is diluted, to prepare the propane oil solution of a series of concentration, under being placed in ml headspace bottle uniform temperature, balance a period of time, get head space gases in bottle and carry out head space gas chromatography, record peak area, drawing standard curve; Again by the testing sample of identical amount, under the same conditions, carry out head space gas chromatography, record peak area, contrasts above-mentioned typical curve, obtains the content of propane in head space gases; Finally be converted to the content of propane in testing sample.
Above-mentioned purpose of the present invention is realized by following steps: the detection method of dissolvent residual in Propane fluid extraction product, carries out according to following step:
(1) preparation of standard reserving solution:take not containing the product oil quality m of propane 1(20.0000 ~ 200.0000 g), propane gas is passed into 10 ~ 60 min in this oil, wherein preferred 20 ~ 40 min, and rear stopping passes into propane gas, then ambient-temp-stable 12 ~ 96 h, and wherein preferably after 48 ~ 84 h, the quality again weighing oil is m 2, the weight of increase is the quality passing into propane gas, obtains the concentration of propane in oil:
X 1=1000(m 2-m 1)/?m 1
In formula:
X 1--the concentration of propane in oil, unit is milligram every gram (mg/g);
M 1--not containing the quality of propane product oil, unit is gram (g);
M 2--quality oily after passing into propane, unit is gram (g).
(2) preparation of series standard solution:pipette storing solution stable in the step (1) that quality is m ' in the tool plug ml headspace bottle of clean drying, close plug, obtains the quality of propane in product oil (mg): m ' × X 1, in this bottle, add the product oil not containing propane is m(5.00 ~ 50.00g to oily quality), close plug, mixed preparing obtains the titer of a series of different propane concentration, and concentration is (m ' × X 1)/m
In formula:
M '--pipette the amount of propane standard reserving solution, unit is gram (g);
M--is used for the oil sample amount of gas chromatographic detection, and unit is gram (g).
(3) head space gas chromatography:by the fat solution of the different propane concentrations of (m) identical in quality in step (2), balance 10 ~ 60 min is stirred with the rotating speed of 500 rpm in 40 ~ 70 DEG C of thermostat water baths, insertion microsyringe or syringe pipette gasification bottle top tank air 100 μ L immediately, carry out head space gas chromatography, write down peak area, take peak area as ordinate, propane concentration is horizontal ordinate, drawing standard curve; Wherein GC conditions is: preferred column HP-PLOT Al 2o 3-S(15m*0.53 mm*15.00 μm), flame ionization ditector (FID), column temperature 40 ~ 100 DEG C, the temperature of vaporizer and detecting device 150 ~ 250 DEG C, carrier gas (N 2) 7.2 mL/min, hydrogen 50 mL/min, air 500 mL/min, the testing sample pipetting (m) identical in quality is deposited in the tool plug ml headspace bottle of volume same as described above, close plug, under the same conditions, carries out head space gas chromatography, write down the peak area (multiple chromatographic peak normalization method) that component is measured, contrast standard opisometer calculates propane content in testing sample (mg/kg): X=1000X 2
In formula:
X 2--the content of propane in testing sample, unit is milligram every gram (mg/g);
The content of propane in X--testing sample, unit is milligrams per kilogram (mg/kg).
(4) evaluation of method accuracy:by head space equilibrium condition and the GC conditions of step (3), 6 parallel replications are carried out to testing sample (oil and fat product of propane extraction), calculates dissolvent residual in sample according to typical curve, and calculate relative standard deviation (RSD)≤5.5%; Again this sample is carried out recovery of standard addition test, add the standard items (high, normal, basic concentration) of three levels, average recovery of standard addition is 95 ~ 110%, RSD is 1 ~ 5.5%.
The product oil not containing propane of the present invention refers to that same oil plant or natural products adopt No. 6 solvents, sherwood oil, supercritical COs 2or the grease that the extraction such as milling process obtains, or the product oil that Propane extracts is carried out 100 DEG C of heating 12 ~ 24 h, drain propane wherein.
Advantage of the present invention:
(1) the present invention gives sufficient inflationtime and suitable stable standing time to the product oil not containing propane and weighs accurately, product oil is absorbed well to propane calibrating gas dissolve each other and reach certain balance, overcoming propane calibrating gas is injected directly in grease, the deficiency of its dissolubility and poor stability, improves the accuracy of propane residue detection;
(2) the present invention adopts the oil same with oil phase to be measured to be matrix oil, propane is identical with the Interaction Force of oil to be measured with matrix oil, there is identical adsorption-desorption mobile equilibrium, therefore when headspace gas chromatography sample introduction, the final equilibrium system of propane oil solution does not change, and the experimental data recorded is accurate;
(3) content that the present invention adopts headspace gas chromatography to detect propane in valuable grease has that cost is low, easy and simple to handle, specificity is strong and pollute the advantages such as little to instrument system.
Accompanying drawing explanation
Fig. 1 is that in example 1, concentration is the propane soybean embryo fat/oil standard solution gas chromatogram of 0.0021 mg/g,
The soybean embryo fat/oil product gas chromatogram of propane extraction to be measured in Fig. 2 example 1,
Propane typical curve obtained in Fig. 3 example 1.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
embodiment 1
Get commercially available No. 6 solvent-extracted soybean embryo fat/oil 50.0000 g, the 150ml loading homemade clean dried constant weight ventilates in bottle (comprising plastic bottle with cover, draft tube and gas outlet).Propane calibrating gas is stored in steel cylinder, the valve controlling flow is had above steel cylinder, communicate with the external world with rubber tube, separately get one section of rubber tube to be communicated with the rubber tube of steel cylinder by emulsion tube, gross mass 110.3620 g of oil and air-breather, open cylinder valve, propane calibrating gas is slowly passed in product oil, valve-off after 0.5 h, the gross mass weighing oil solution and air-breather is 111.3323 g, standing at room temperature places 72h, again weigh the gross mass of product oil and air-breather, its steady quality does not change in 110.3624(1h), the quality relatively increased before and after ventilation is the quality of fat absorption propane, thus obtain the Standard Stock solutions that concentration is 0.0080mg/g, get the Standard Stock solutions of certain mass and soybean embryo fat/oil mixed diluting quantitatively to 10.00 g not containing propane, obtained propane concentration of standard solution is followed successively by 0.0041 mg/g, 0.00031 mg/g, 0.0021 mg/g, 0.0010 mg/g, 0.0008 mg/g, 0.0004 mg/g, 0.0002 mg/g, and by its series standard solution close plug in 135 mL ml headspace bottle, balance 15 min is stirred with the rotating speed of 500 rpm respectively in 50 DEG C of thermostat water baths, from ml headspace bottle, 100 μ L top tank airs are extracted immediately with microsyringe, pass through gas chromatographic analysis, write down component peaks area, with peak area, linear regression is carried out to propane concentration, obtaining regression equation is y=565377x-57.101, correlation coefficient r=0.9991, the range of linearity is 0.0002 ~ 0.0041 mg/g.Get the soybean germ oil product (laboratory obtains) of 10.00 g Propane extractions, close plug in 135 mL ml headspace bottle, water bath with thermostatic control 15 min at 50 DEG C, from bottle, extract 100 μ L with micro syringe immediately and carry out analysis headspace gas chromatography, write down each component peaks area, comparison typical curve, the residual quantity calculating propane in the soybean embryo fat/oil of Propane extraction is 0.22mg/kg.
Wherein gas chromatography reference conditions:
Chromatographic column: HP-PLOT Al 2o 3-S (15m*0.53mm*15.00 μm)
Detecting device: FID
Column temperature: 70 DEG C
Temperature of vaporization chamber: 180 DEG C
Detector temperature: 210 DEG C
Carrier gas (N 2): 7.2 mL/min
Hydrogen: 50 mL/min
Air: 500 mL/min
embodiment 2
Get supercritical CO 2wheat-germ oil 100.0000 g of extraction, the 150ml loading homemade clean dried constant weight ventilates in bottle.Propane calibrating gas is stored in steel cylinder, the valve controlling flow is had above steel cylinder, communicate with the external world with rubber tube, separately get one section of rubber tube to be communicated with the rubber tube of steel cylinder by emulsion tube, gross mass 160.3453 g of oil and air-breather, open cylinder valve, propane calibrating gas is slowly passed in product oil, valve-off after 1 h, the gross mass weighing oil and air-breather is 161.9173 g, standing at room temperature places 84h, again weigh the gross mass of product oil and air-breather, its steady quality does not change in 160.3467(1h), the quality relatively increased before and after ventilation is the quality of fat absorption propane, thus obtain the Standard Stock solutions that concentration is 0.0140mg/g, get the Standard Stock solutions of certain mass and wheat-germ oil mixed diluting quantitatively to 10.00 g not containing propane, obtained propane concentration of standard solution is followed successively by 0.0070 mg/g, 0.0053 mg/g, 0.0035 mg/g, 0.0028 mg/g, 0.0014 mg/g, 0.0006 mg/g, 0.0003 mg/g, 0.0001 mg/g, and by its series standard solution close plug in 135 mL ml headspace bottle, balance 15 min is stirred with the rotating speed of 500 rpm respectively in 50 DEG C of thermostat water baths, from ml headspace bottle, 100 μ L top tank airs are extracted immediately with microsyringe, pass through gas chromatographic analysis, write down peak area, with peak area, linear regression is carried out to propane concentration, obtaining regression equation is y=507627x-36.541, correlation coefficient r=0.9997, the range of linearity is 0.0001 ~ 0.0070 mg/g.Get the wheat embryo oil product (commercially available) of 10.00 g Propane extractions, close plug in 135 mL ml headspace bottle, at 50 DEG C of water bath with thermostatic control 15 min, from bottle, extract 100 μ L with micro syringe immediately and carry out analysis headspace gas chromatography, write down component peaks area, the above-mentioned typical curve of comparison, calculates solvent residual amount in the wheat-germ oil of Propane extraction and does not detect.
Wherein gas chromatography reference conditions:
Chromatographic column: HP-PLOT Al 2o 3-S (15m*0.53mm*15.00 μm)
Detecting device: FID
Column temperature: 40 DEG C
Temperature of vaporization chamber: 150 DEG C
Detector temperature: 250 DEG C
Carrier gas (N 2): 7.2 mL/min
Hydrogen: 50 mL/min
Air: 500 mL/min
embodiment 3
Get commercially available No. 6 solvent-extracted rice bran oil 50.0000 g, the 150ml loading homemade clean dried constant weight ventilates in bottle (comprising plastic bottle with cover, draft tube and gas outlet).Propane calibrating gas is stored in steel cylinder, the valve controlling flow is had above steel cylinder, communicate with the external world with rubber tube, separately get one section of rubber tube to be communicated with the rubber tube of steel cylinder by emulsion tube, gross mass 110.3620 g of oil and air-breather, open cylinder valve, propane calibrating gas is slowly passed in product oil, valve-off after 0.5 h, the gross mass weighing oil solution and air-breather is 111.3329 g, static placement 72 h of difference under room temperature, again weigh the gross mass of product oil and air-breather, its steady quality does not change in 110.3625(1h), the quality relatively increased before and after ventilation is the quality of fat absorption propane, thus obtain the Standard Stock solutions that concentration is 0.0100mg/g, the Standard Stock solutions getting certain mass respectively with rice bran oil mixed diluting quantitatively to 10.00 g not containing propane, obtained propane concentration of standard solution is followed successively by 0.0050 mg/g, 0.00038 mg/g, 0.0025 mg/g, 0.0020 mg/g, 0.0010 mg/g, 0.0005 mg/g, 0.0003 mg/g, and by its series standard solution close plug in 135 mL ml headspace bottle, balance 15 min is stirred with the rotating speed of 500 rpm respectively in 50 DEG C of thermostat water baths, from ml headspace bottle, 100 μ L top tank airs are extracted immediately with microsyringe, pass through gas chromatographic analysis, write down component and record peak area, with peak area, linear regression is carried out to propane concentration, obtaining regression equation is y=565468x-168.261, correlation coefficient r=0.9991, the range of linearity is 0.0003 ~ 0.0050 mg/g.Get the rice bran oil product (laboratory obtains) of 10.00 g Propane extractions, close plug in 135 mL ml headspace bottle, water bath with thermostatic control 15 min at 50 DEG C, from bottle, extract 100 μ L top tank airs with micro syringe immediately and carry out analysis headspace gas chromatography, write down component peaks area, the above-mentioned typical curve of comparison, calculates solvent residual amount in the rice bran oil of Propane extraction and does not detect.
Wherein gas chromatography reference conditions:
Chromatographic column: HP-PLOT Al 2o 3-S (15m*0.53mm*15.00 μm)
Detecting device: FID
Column temperature: 70 DEG C
Temperature of vaporization chamber: 180 DEG C
Detector temperature: 210 DEG C
Carrier gas (N 2): 7.2 mL/min
Hydrogen: 50 mL/min
Air: 500 mL/min.

Claims (1)

1.亚临界丙烷流体萃取产品中溶剂残留的检测方法,其特征在于按照下述步骤进行: 1. the detection method of residual solvent in the subcritical propane fluid extraction product is characterized in that carrying out according to the following steps: (1)标准储备液的配制:称取不含丙烷的成品油质量m1,将丙烷气体通入该油中10~60 min,后停止通入丙烷气体,然后室温稳定12~96 h,再次称量油的质量为m2,增加的重量即为通入丙烷气体的质量,得到丙烷在油中的浓度: (1) Preparation of standard stock solution: Weigh the mass m 1 of the refined oil without propane, inject propane gas into the oil for 10-60 min, then stop feeding propane gas, then stabilize at room temperature for 12-96 h, and again Weigh the mass of the oil as m 2 , the increased weight is the mass of the propane gas, and the concentration of propane in the oil is obtained: X1=1000(m2-m1)/ m1 X 1 =1000(m 2 -m 1 )/ m 1 式中: In the formula: X1――丙烷在油中的浓度,单位为毫克每克; X 1 - the concentration of propane in the oil, the unit is milligram per gram; m1――不含丙烷成品油的质量,单位为克; m 1 - the mass of refined oil without propane, in grams; m2――通入丙烷后油的质量,单位为克; m 2 - the mass of the oil after passing through the propane, the unit is gram; (2)系列标准溶液的配制:移取质量为m′的步骤(1)中稳定的储备液到清洁干燥的具塞顶空瓶中,密塞,得到丙烷在成品油中的质量:m′×X,向该瓶中加入不含丙烷的成品油至油的质量为m,密塞,混合配制得到一系列不同丙烷浓度的标准液,浓度为(m′×X1)/m (2) Preparation of a series of standard solutions: pipette the stable stock solution in step (1) with a mass of m′ into a clean and dry headspace bottle with a stopper, and seal it tightly to obtain the mass of propane in the product oil: m′ ×X 1 , add refined oil without propane to the bottle until the mass of the oil is m, seal it tightly, mix and prepare a series of standard solutions with different propane concentrations, the concentration is (m′×X 1 )/m 式中: In the formula: m′――移取丙烷标准储备液的量,单位为克; m′——the amount of propane standard stock solution pipetted, in grams; m――用于气相色谱检测的油样量,单位为克; m - the amount of oil sample used for gas chromatography detection, in grams; (3)顶空气相色谱分析:将步骤(2)中质量相同的不同丙烷浓度的油脂溶液,在40~70 ℃恒温水浴锅中以500 rpm的转速搅拌平衡10~60 min,立即插入微量进样器或注射器移取气化瓶上层气体100 μL,进行顶空气相色谱分析,记下峰面积,以峰面积为纵坐标,丙烷浓度为横坐标,绘制标准曲线;移取质量相同的待测样品存放于与上述相同体积的具塞顶空瓶中,密塞,在相同条件下,进行顶空气相色谱分析,记下组分测量的峰面积,多个色谱峰用归一化法,对比标准曲线计算出待测样品中丙烷含量,单位为毫克每克:X=1000X2 (3) Headspace gas chromatographic analysis: Stir the fat solutions with the same quality and different propane concentrations in step (2) in a constant temperature water bath at 40-70 °C at a speed of 500 rpm for 10-60 min, and immediately insert a micropipette into the Pipette 100 μL of the gas in the upper layer of the gasification bottle with a sampler or syringe, conduct headspace gas chromatography analysis, record the peak area, take the peak area as the ordinate, and the propane concentration as the abscissa, draw a standard curve; Store the sample in a headspace bottle with a stopper of the same volume as above, and seal it tightly. Under the same conditions, carry out headspace gas chromatography analysis, record the peak area of the component measurement, use the normalization method for multiple chromatographic peaks, and compare The standard curve calculates the content of propane in the sample to be tested, in milligrams per gram: X=1000X 2 式中: In the formula: X2――待测样品中丙烷的含量,单位为毫克每克; X 2 - the content of propane in the sample to be tested, in milligrams per gram; X――待测样品中丙烷的含量,单位为毫克每千克; X - the content of propane in the sample to be tested, in milligrams per kilogram; (4)方法准确性的评价:对待测样品即丙烷萃取的油脂产品按步骤(3)的顶空平衡条件和气相色谱条件进行6次平行重复测定,根据标准曲线计算出样品中溶剂残留,并计算相对标准偏差RSD≤5.5%;再将该样品进行加标回收率试验,添加三个水平的标准品即高中低浓度,平均加标回收率为95~110%,RSD为1~5.5%; (4) Evaluation of the accuracy of the method: The sample to be tested, that is, the oil product extracted by propane, was measured in parallel for 6 times according to the headspace equilibrium conditions and gas chromatography conditions of step (3), and the solvent residue in the sample was calculated according to the standard curve, and Calculate the relative standard deviation RSD ≤ 5.5%; then carry out the standard addition recovery test on the sample, add three levels of standard products, that is, high, middle and low concentrations, the average standard recovery rate is 95~110%, and the RSD is 1~5.5%; 其中气相色谱条件为:色谱柱HP-PLOT Al2O3-S 15m*0.53 mm*15.00 μm,氢火焰离子化检测器FID,柱温40~70 ℃,汽化室和检测器的温度150~250 ℃,载气N27.2 mL/min,氢气50 mL/min,空气500 mL/min。 The gas chromatography conditions are: HP-PLOT Al 2 O 3 -S 15m*0.53 mm*15.00 μm chromatographic column, hydrogen flame ionization detector FID, column temperature 40-70 ℃, vaporization chamber and detector temperature 150-250 ℃, carrier gas N 2 7.2 mL/min, hydrogen 50 mL/min, air 500 mL/min.
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CN102323353A (en) * 2011-08-16 2012-01-18 上海新先锋药业有限公司 Method for detecting organic solvent residues in liposome medicines

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