Sediaan farmasi yang beredar di perdagangan seringkali berbentuk kombinasi campuran berbagai zat berkhasiat, seperti metampiron dan diazepam. Meningkatnya produksi obat-obat ini perlu diimbangi dengan peningkatan pengawasan mutu, agar obat yang beredar tersebut dapat dijamin keamanan dan khasiatnya. Oleh sebab itu diperlukan metode analisis yang akurat, jika memungkinkan sederhana dan murah, untuk menganalisis kandungan sediaan kombinasi metampiron dan diazepam tersebut. Salah satu metode analisis yang murah dan sederhana adalah KLT video densitometri. Tujuan dari penelitian ini untuk memvalidasi metode KLT video densitometri dalam penetapan kadar sediaan kombinasi tablet metampiron dan diazepam. Pengujian pemisahan menggunakan plat KLT GF254, plat ditotol senyawa aktif dan dikembangkan menggunakan fase gerak metanol:n-butanol (1:5, V/V) dengan penambahan amonia sebanyak 3 tetes. Visualisasi, perekaman bercak dan analisis kromatogram menggunakan seperangkat alat video densitometri. Hasil pengujian uji kesesuaian sistem diperoleh nilai Rf metampiron dan diazepam berturut-turut adalah 0,3 dan 0,8. Pembuatan sampel simulasi dilakukan dengan memvariasikan kadar metampiron dan diazepam. Nilai-nilai parameter dari validasi metode analisis yang dikembangkan yaitu untuk metampiron dengan rentang 90-115 bpj diperoleh nilai koefisien korelasi (r)=0,998; BD dan BK=1,755 dan 5,849 bpj; % recovery 100,203; 99,392 dan 100,649%, RSD (interday) 100%=1,031%. Sedangkan nilai parameter untuk diazepam dengan rentang 80–105 bpj, diperoleh nilai koefisien korelasi (r)=0,998; BD dan BK=2,102 bpj dan 7,006 bpj; % recovery 100,261; 99,622; dan 100,409%, RSD (interday) 100%=1,517%. Diperoleh hasil penetapan kadar yaitu metampiron dan diazepam berturut-turut adalah sebesar 100,358 dan 100,918%. Nilai-nilai parameter validasi tersebut memenuhi syarat yang telah ditetapkan sehingga metode KLT video densitometri layak digunakan untuk penetapan kadar metampiron dan diazepam. Pharmaceutical dosage forms that circulate in the trade are often a mixture of different combination of active substances. Due to increasing production of these drugs need to be offset by increasing the quality control, so that the drug circulation can be guaranted safely and effectively. It therefore requires both an accurate analysis method and simple and cheap to analyze the contents in combination of methampyron and diazepam. One of the simple and cheap methods is TLC video densitometry. The aim of the research was validating TLC video densitometry in determinating content of combination of methampyron and diazepam. The separation was performed by using a TLC plate GF254, the plate that were apllied and developed with active compounds using a mobile phase of methanol:n-butanol (1:5, V/V) and 3 drops of ammonia. The spot was visualized, recorded spotting and chromatogram analyzed by using a set of densitometry video tools. The conformance system results showed that the value of Rf for methampyron and diazepam of 0.3 and 0.8, respectively. Formulation of sample simulation was carried out by varying concentrations of methampyron and diazepam. The parameters of the developed analytical validation methods in the range of 90-115 ppm of methampyron obtained correlation coefficient (r) of 0.998; limit of detection and limit of quantity of 1.755 and 5.849 ppm, respectively; % recovery of 100.203; 99.392; and 100.649%; % of RSD (interday) 100% of 1.031%, while the parameter for diazepam with a range of 80-105 ppm, the value of the correlation coefficient (r) of 0.998; limit of detection and limit of quantity of 2.102 and 7.006 ppm, respectively; % recovery were 100.26; 99.622, and 100.409%, % of RSD (interday) 100% of 1.517. The result showed that the content of methampyron and diazepam were 100.358 and 100.918%, respectively. It showed that the values of the parameter validation are eligible, so that TLC video densitometry method was feasible to use for determination of methampyron and diazepam.