Abstract: teflon borate can be used as resin finishing catalyst in textile printing and dyeing industry. Used for non-metallic refining flux, coating, fluorizer, chemical reagent, electrochemical engineering, etc. It is also used as an organic reagent and medicine intermediate.
An ion chromatography method for simultaneous determination of four ion tetrafluoroborate, p-methylbenzene sulfonic acid, sulfuric acid and 1, 4-butadisulfonic acid in drug synthesis was established. The results show that the separation degree of the four ions is good, the sensitivity is high, the linear range is between 3 and 150mg/L, the correlation coefficient is above 0.999, the precision is less than 1%, and the recovery rate is between 99.1% and 105.3%. Applicable to the determination of actual samples.
P-methylbenzene sulfonic acid is widely used in synthesis of stabilizers for pharmaceutical, pesticide and polymerization reactions as well as catalysts for organic synthesis (esters, etc.). Also used as medicine, paint intermediates and resin curing agents.
1, 4-butyldisulfonic acid is one of the raw materials for synthesis of adenosine butylsulfonic acid, which is a compound salt formed by adenosine methionine and butyldisulfonic acid at a ratio of 1:1.65. 1, 4 - succinic acid adenosine methionine, the active ingredient for adenosine methionine cation, 1, 4 - butylene sulfonic acid root as the role of anion and its matching to stabilize its structure, does not have pharmacological activities [1]. Adenosine butylsulfonic acid can be used to treat intrahepatic cholestasis and intrahepatic cholestasis during pregnancy before and after cirrhosis [2].
These 3 kinds of ions and sulfuric acid root ions often need quantitative determination in pharmaceutical synthesis. The ultraviolet spectrophotometry needs to select the maximum absorption wavelength of the ions. If the ions are measured at the same time, the sensitivity is not high. The simultaneous separation and determination of the above three ions and sulfuric acid root ions can be achieved by ion chromatography, with wide linear range, no pollution, good reproducibility and high accuracy of sample determination.
1. Experiment
1.1 main instruments and reagents
Ion chromatograph: CIC-100, Qingdao shenghan chromatographic technology co., LTD.
Anionic chromatographic column: shodex90-4e, Shodex, Japan;
Sodium carbonate, sodium bicarbonate: analytical purity;
Leaching solution: 1.8mmol/ lna2co3-1.7mmol /LNaHCO3 mixed solution, said to take 0.190g sodium carbonate and 0.1428g sodium bicarbonate, with degassing water capacity to 1000mL;
Four fluoboric acid sodium, the methyl benzene sulfonic acid, 1, 4 - butylene sulfonic acid, sodium sulfate liquid reserves: respectively according to four fluoboric acid sodium, the methyl benzene sulfonic acid, 1, 4 - butylene sulfonic acid, sodium sulfate, 0.1, 0.1, 0.1265 and 0.1479 g in 100 ml volumetric flask and with the capacity to scale the deionized water;
The experimental water is deionized water.
1.2 chromatographic conditions
Leaching solution: 1.8mmol/ lna2co3-1.7mmol/lnahco3-5% acetonitrile, flow rate 1.0mL/min; Detector: conductance detector; The sampling amount: 100 is the same thing as L.
2 the results
2.1 selection of chromatographic conditions
Respectively test the tendency for 1.8 / LNa2CO3 1.7 tendency LNaHCO3 plus 3%, 5%, 8% and 10% acetonitrile under the condition of chromatography separation, results show that when adding 3% acetonitrile in methyl benzene sulfonic acid and sulfuric acid root overlap, when adding 8% and 10% acetonitrile, BF4 overlap with the methyl benzene sulfonic acid, and adding acetonitrile was 5%, the ratio of volume degree of separation between ions are above 1.5, so the experiment choice tendency for 1.8 / LNa2CO3 1.7 tendency LNaHCO3-5% acetonitrile as eluent.
2.2 selection of rinsing fluid velocity
The separation of ions in the range of 0.6 ~ 1.2ml /min was tested. When the flow rate of 1.0mL/min is adopted, it can not only save time for fast separation but also meet the separation requirements. Therefore, the experimental choice of rinsing liquid flow rate is 1.0mL/min.
2.3 work curve and detection limit
The concentrations of the four ions were respectively 5mg· l-1 teflon borate, 50mg· l-1 p-toluene sulfonate, 42-40mg· l-1, 1, 4-butadisulfonate, 150mg· l-1. The solution is then diluted 2 times, 4 times, 20 times and 100 times. The linear equation, linear range, correlation coefficient and detection limit of the four ions measured are listed in table 1.
Table 14 linear equation, linear range, correlation coefficient, detection limit of 14 kinds of ions
The detection limit of the linear range/mg· l-1 correlation coefficient of the ionic linear equation/mg· l-1 4-butyldisulfonate root Y=-7.881 * 104 4.218 * 104X3 ~ 1500.99950.039
Note: X is the ion concentration and Y is the chromatographic peak area.
2.4 sample determination
C18 activation and regeneration: 5mL chromatography-grade methanol was first used for washing, followed by 10ml secondary deionized water.
Sample under test (provided by a pharmaceutical factory, divided into 1 # and 2 #, 1 # for the methyl benzene sulfonic acid drugs, 2 # 1.4 - butyl disulfonic acid drugs) with secondary water dissolved, after using C18 column into the ion chromatography were analyzed.
Table 21 original sample results
The content of ingredients to be measured is mg/kg teflon borate 23421.4- butyldisulfonate ND p-methyl benzene sulfonate root 372989so42-226083
Note: ND is not detected. Table 32 original sample results
The content of ingredients to be measured is mg/kg teflon borate ND p-methyl benzene sulfonate ND1.4- butyl disulfonate root 509386so42-4769
Note: ND is not detected.
3 conclusion
The tetrafluoroborate and p-toluene sulfonate were separated and determined simultaneously by ion-chromatographic conductometry
