During a recent investigation of the organotin-contaminated lard samples, a simple method was developed by direct Grignard pentylation of lard samples and capillary gas chromatography with flame photometric detection using quartz surface-induced tin emission. Using HP-1 capillary column with temperature programming and FPD detector, pentylated tri-, di-, monometyltin, dioctyltin and Sn(IV) can be base-line separated and detected within 20 min. The analysis of pentylated tin compounds by GC-MS confirmed the existence of methyltins and inorganic tin in lard samples, which was agreeable with the results obtained by GC-FPD. The content of organotin compounds was calculated by internal standard method in which methyltripropyltin (MeSnPr3) acted as internal standard. The results showed that these samples were heavily contaminated with mg/g levels of dimethyltin, microg/g levels of tri- and monomethyltin. Among them, one sample contained mg/g level of dioctyltin and one contained a little of inorganic form of Sn(IV). The recoveries of tri-, di- and monomethyltin were 95.7%, 105.5% and 105.7%, respectively.