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目的建立用外标法测定尼可地尔中残留溶剂的气相色谱法。方法采用DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷);规格:30m×0.53mm×3.0μm;载气为:氮气;检测器:FID(氢火焰离子化检测器);柱温:40℃保持5min,然后以50℃/min升温至240℃,并保持3min;进样口温度:120℃;检测器温度:250℃;载气流速:4.0ml/min;分流比:15;柱压:20kp;计算方法:外标法。结果乙醇在线性范围内2.0～200.0μg·ml-1,相关系数R=0.99999;丙酮在线性范围内2.0～200.0μg·ml-1,相关系数R=0.99917;甲苯在线性范围内0.9～90.0μg·ml-1,相关系数R=0.99995;各溶剂线性关系良好。三种残留溶剂乙醇、丙酮和甲苯平均回收率依次为97.0、98.6%和99.7%。结论本测定方法简便快速,灵敏度高,准确度好,可用于尼可地尔残留溶剂的测定。
Objective To establish a gas chromatographic method for the determination of residual solvents in Nicorandil by external standard method. The method uses DB-624 (6% cyanopropylphenyl-94% dimethylpolysiloxane); the specification is 30m × 0.53mm × 3.0μm; the carrier gas is nitrogen; the detector is FID (hydrogen flame ionization Detector); column temperature: 40 ° C for 5 min then ramp to 240 ° C at 50 ° C / min and hold for 3 min; inlet temperature: 120 ° C; detector temperature: 250 ° C; carrier gas flow rate: 4.0 ml / min ; Split ratio: 15; Column pressure: 20kp; Calculation method: external standard method. Results The linear range of ethanol was 2.0 ~ 200.0μg · ml-1, the correlation coefficient was 0.99999. The linear range of acetone was 2.0 ~ 200.0μg · ml-1, the correlation coefficient was 0.99917. The linear range of toluene was 0.9 ~ 90.0μg · Ml-1, correlation coefficient R = 0.99995; The linearity of each solvent is good. The average residual recoveries of ethanol, acetone and toluene were 97.0, 98.6% and 99.7%, respectively. Conclusion The method is simple, rapid, sensitive and accurate. It can be used for the determination of residual solvents in nicorandil.